CN112067677A - Silver-antimony alloy solid pH response electrode and preparation method and application thereof - Google Patents
Silver-antimony alloy solid pH response electrode and preparation method and application thereof Download PDFInfo
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- CN112067677A CN112067677A CN202010941406.5A CN202010941406A CN112067677A CN 112067677 A CN112067677 A CN 112067677A CN 202010941406 A CN202010941406 A CN 202010941406A CN 112067677 A CN112067677 A CN 112067677A
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Abstract
A silver-antimony alloy solid pH response electrode and a preparation method and application thereof relate to the field of metal electrodes and solve the problems of poor pH response stability, low strength, brittleness, poor corrosion resistance and short service life of the existing antimony pH response electrode. The silver-antimony alloy solid pH response electrode is made of a silver-antimony alloy material, wherein antimony accounts for wt% of the silver-antimony alloy material1% is: 27 percent to wt1Percent is less than 100 percent, and the mass percent of silver is wt2% is: 0 < wt2The percentage is less than or equal to 73 percent. Compared with the existing antimony pH response electrode, the silver-antimony (Ag-Sb) alloy solid pH response electrode has better performance, better pH response stability, better mechanical property, stronger corrosion resistance and longer service life.
Description
Technical Field
The invention relates to the technical field of metal electrodes, in particular to a silver-antimony alloy solid pH response electrode and a preparation method and application thereof.
Background
The pH value is one of the most common chemical properties, can reflect water quality, food quality and the like, and has important practical monitoring significance in the fields of water quality safety monitoring, environmental protection, food safety, medical health and the like. At present, the detection of pH value is realized by a potential electrochemical sensor in the widest application. Common pH test procedures: the response electrode and the reference electrode are utilized to form a galvanic cell, a potential difference (open circuit potential) between the two electrodes is tested through an instrument, and the conversion between the detected potential and the pH value of the solution is realized according to the standard calibration relation of the electrodes in a standard pH buffer solution, so that the purpose of testing the pH value is achieved.
The existing pH response electrode comprises a glass electrode and a metal solid electrode, wherein the glass electrode is not suitable for harsh working conditions such as high voltage and the like due to the fragile glass bubbles, and the metal solid electrode is widely applied to harsh environments such as high voltage resistance and the like due to good mechanical properties of the metal solid electrode.
Antimony (Sb) electrodes have been successfully commercialized as a metal solid-state pH-responsive electrode and are mainly used in industrial environments. However, the main problems of the antimony pH-responsive electrode are: poor pH response stability, low strength, brittleness, poor corrosion resistance, short service life and the like, and the existence of the problems greatly limits the wider application of the composite material.
Disclosure of Invention
In order to solve the problems of poor pH response stability, low strength, brittleness, poor corrosion resistance and short service life of the conventional antimony pH response electrode, the invention provides the silver-antimony alloy solid pH response electrode, and the preparation method and the application thereof.
The technical scheme adopted by the invention for solving the technical problem is as follows:
the silver-antimony alloy solid pH response electrode is made of a silver-antimony alloy material, wherein antimony accounts for wt% of the silver-antimony alloy material1% is: 27 percent to wt1Percent is less than 100 percent, and the mass percent of silver is wt2% is: 0 < wt2％≤73％。
In a preferred embodiment, the mass percent wt of antimony in the silver-antimony alloy material1% is: 46 percent to wt1Percent is less than 100 percent, and the mass percent of silver is wt2% is: 0 < wt2％≤54％。
In a more preferred embodiment, the silver-antimony alloy material has an antimony content of 75% by mass and a silver content of 25% by mass.
The preparation method of the silver-antimony alloy solid pH response electrode comprises the following steps:
step one, selecting silver powder and antimony powder as raw materials, weighing the silver powder and the antimony powder which meet the mass percentage, and grinding and mixing the silver powder and the antimony powder uniformly;
step two, preparing a silver-antimony alloy electrode bar;
and step three, grinding one end of the silver-antimony alloy electrode bar to be flat as a pH response surface, and welding the other end of the silver-antimony alloy electrode bar with a lead to prepare the silver-antimony alloy solid pH response electrode.
As a preferred embodiment, in the first step, the silver powder is high-purity silver powder, and the antimony powder is high-purity antimony powder.
And step two, preparing the silver-antimony alloy electrode rod by using a high-temperature molten metal casting method and a glass tube as a casting mould, or preparing the silver-antimony alloy electrode film by using a magnetron sputtering method, or preparing the silver-antimony alloy electrode film by using a high-temperature chemical vapor deposition method.
In a preferred embodiment, in the second step, the parameters of the high-temperature molten metal casting method are as follows: the melting temperature is more than or equal to 670 ℃, the heat preservation time is 4-6h, and the silver-antimony alloy electrode rod is obtained after the furnace is naturally cooled to the room temperature.
In a more preferred embodiment, the melting temperature is 680 ℃ and the holding time is 5 hours.
The silver-antimony alloy solid pH response electrode is applied to preparing an all-solid-state composite pH sensor, and the composite pH sensor is prepared by compounding the silver-antimony alloy solid pH response electrode and a reference electrode.
As a preferred embodiment, the reference electrode is: a solid silver/silver chloride reference electrode, a saturated calomel reference electrode, or a mercury/mercury oxide reference electrode.
The invention has the beneficial effects that:
compared with the existing antimony pH response electrode, the silver-antimony (Ag-Sb) alloy solid pH response electrode has better performance, better pH response stability, better mechanical property, stronger corrosion resistance and longer service life.
Drawings
FIG. 1 is a sensitivity test chart of a silver-antimony alloy solid pH response electrode.
FIG. 2 is a stability test chart of a silver-antimony alloy solid pH response electrode.
FIG. 3 is a corrosion resistance test chart of a silver-antimony alloy solid pH response electrode under the condition of pH 6.86. In fig. 3, a is actually measured electrochemical alternating current impedance data, and in fig. 3, b is an alternating current impedance nyquist plot obtained by fitting the data of a in fig. 3 through ZView software.
FIG. 4 is a corrosion resistance test chart of a silver-antimony alloy solid pH response electrode under the condition of pH 9.18. In fig. 4, a is actually measured electrochemical alternating current impedance data, and in fig. 4, b is an alternating current impedance nyquist plot obtained by fitting the data of a in fig. 4 through ZView software.
Detailed Description
The silver-antimony alloy solid pH response electrode is made of a silver-antimony alloy material, wherein antimony accounts for wt% of the silver-antimony alloy material1% is: 27 percent to wt1Percent is less than 100 percent, and the mass percent of silver is wt2% is: 0 < wt2％≤73％。
Preferably, in the silver-antimony alloy material, the mass percent wt of antimony1% is: 46 percent to wt1Percent is less than 100 percent, and the mass percent of silver is wt2% is: 0 < wt2％≤54％。
More preferably, in the silver-antimony alloy material, the mass percent of antimony is 75%, and the mass percent of silver is 25%.
The preparation method of the silver-antimony alloy solid pH response electrode mainly comprises the following steps:
step one, selecting high-purity silver powder (with the purity of 99.5%) and high-purity antimony powder (with the purity of 99.9%) as raw materials, weighing the silver powder and the antimony powder which meet the mass percentage, and fully grinding the silver powder and the antimony powder in a mortar to uniformly mix the silver powder and the antimony powder.
Step two, preparing the silver-antimony alloy electrode bar by adopting a high-temperature molten metal casting method and taking a glass tube as a casting mould: the melting temperature is more than or equal to 670 ℃, the heat preservation time is 4-6h, and the silver-antimony alloy electrode rod is obtained after the furnace is naturally cooled to the room temperature.
Preferably, the melting temperature is 680 ℃ and the holding time is 5 h.
The preparation method of the silver-antimony alloy electrode comprises but is not limited to a high-temperature molten metal casting method, and can also adopt the following steps: magnetron sputtering, high-temperature chemical vapor deposition and the like.
And step three, grinding one end of the silver-antimony alloy electrode bar to be flat as a pH response surface, and welding the other end of the silver-antimony alloy electrode bar with a lead to prepare the silver-antimony alloy solid pH response electrode.
The silver-antimony alloy solid pH response electrode is applied to the preparation of a pH composite electrode sensor, and the pH composite electrode sensor is prepared by compounding the silver-antimony alloy solid pH response electrode and a reference electrode. Wherein, the reference electrode is selected from: a solid silver/silver chloride reference electrode, a saturated calomel reference electrode, or a mercury/mercury oxide reference electrode.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
EXAMPLE 1 preparation of silver-antimony alloy solid pH responsive electrode
The silver-antimony alloy solid-state pH response electrode prepared in the embodiment is made of a silver-antimony alloy material, wherein the mass percent of antimony and the mass percent of silver in the silver-antimony alloy material are respectively 75% and 25%.
The preparation method comprises the following specific steps:
(1) the preparation method comprises the steps of selecting high-purity silver powder and high-purity antimony powder as raw materials, weighing the silver powder and the antimony powder which meet the mass percentage, and fully grinding the silver powder and the antimony powder in a mortar to uniformly mix the silver powder and the antimony powder.
(2) Preparing a silver-antimony alloy electrode bar by adopting a high-temperature molten metal casting method and taking a glass tube as a casting mould: the melting temperature is 680 ℃, the heat preservation time is 5 hours, and the furnace is naturally cooled to the room temperature to obtain the silver-antimony alloy electrode bar.
(3) And grinding one end of the silver-antimony alloy electrode bar to be flat as a pH response surface, and welding the other end of the silver-antimony alloy electrode bar with a lead to prepare the silver-antimony alloy solid pH response electrode.
EXAMPLE 2 preparation of silver-antimony alloy solid pH responsive electrode
The silver-antimony alloy solid-state pH response electrode prepared in the embodiment is made of a silver-antimony alloy material, wherein the mass percent of antimony and the mass percent of silver in the silver-antimony alloy material are 46% and 54%.
The preparation method comprises the following specific steps:
(1) the preparation method comprises the steps of selecting high-purity silver powder and high-purity antimony powder as raw materials, weighing the silver powder and the antimony powder which meet the mass percentage, and fully grinding the silver powder and the antimony powder in a mortar to uniformly mix the silver powder and the antimony powder.
(2) Preparing a silver-antimony alloy electrode bar by adopting a high-temperature molten metal casting method and taking a glass tube as a casting mould: the melting temperature is 680 ℃, the heat preservation time is 5 hours, and the furnace is naturally cooled to the room temperature to obtain the silver-antimony alloy electrode bar.
(3) And grinding one end of the silver-antimony alloy electrode bar to be flat as a pH response surface, and welding the other end of the silver-antimony alloy electrode bar with a lead to prepare the silver-antimony alloy solid pH response electrode.
EXAMPLE 3 preparation of silver-antimony alloy solid pH responsive electrode
The silver-antimony alloy solid-state pH response electrode prepared in the embodiment is made of a silver-antimony alloy material, wherein the mass percent of antimony and the mass percent of silver in the silver-antimony alloy material are 36% and 64%, respectively.
The preparation method comprises the following specific steps:
(1) the preparation method comprises the steps of selecting high-purity silver powder and high-purity antimony powder as raw materials, weighing the silver powder and the antimony powder which meet the mass percentage, and fully grinding the silver powder and the antimony powder in a mortar to uniformly mix the silver powder and the antimony powder.
(2) Preparing a silver-antimony alloy electrode bar by adopting a high-temperature molten metal casting method and taking a glass tube as a casting mould: the melting temperature is 680 ℃, the heat preservation time is 5 hours, and the furnace is naturally cooled to the room temperature to obtain the silver-antimony alloy electrode bar.
(3) And grinding one end of the silver-antimony alloy electrode bar to be flat as a pH response surface, and welding the other end of the silver-antimony alloy electrode bar with a lead to prepare the silver-antimony alloy solid pH response electrode.
Test examples Performance testing of silver-antimony alloy solid-State pH-responsive electrodes
1. Sensitivity testing
Open circuit potentials of the silver-antimony alloy solid-state pH response electrodes prepared in examples 1, 2 and 3 in standard buffer pH values of 4.00, 6.86, 7.00, 9.18 and 10.00 were tested using an electrochemical workstation (shanghai chen CHI832D), and a standard linear relationship was drawn using the open circuit potentials and the corresponding pH values to obtain response sensitivities of the respective electrodes, and the results are shown in fig. 1. As can be seen in FIG. 1, each electrode responds with a sensitivity of-0.055V/pH, approaching the Nernst response sensitivity (-0.0591V/pH).
2. Stability test
The open circuit potentials of the silver-antimony alloy solid-state pH responsive electrode prepared in example 1 in the standard buffer pH of 4.00, 7.00, 10.00 were continuously tested using an electrochemical workstation (shanghai chen CHI832D) for 10 hours, and the stability results of the electrode were reflected by the variation of the open circuit potential within 10 hours as shown in fig. 2. As can be seen from FIG. 2, the silver-antimony alloy solid pH responsive electrode prepared in example 1 exhibited excellent potential stability with stability of less than 0.5mV/h, 0.3mV/h, 0.4mV/h in standard buffer pH 4.00, 7.00, 10.00, respectively.
3. Test of Corrosion resistance
The corrosion resistance of each electrode at a standard buffered pH of 6.86, pH 9.18 was tested using an electrochemical workstation (shanghai chen hua CHI 760E).
The specific implementation method comprises the following steps:
the corrosion resistance of each electrode in the solution is reflected by a nyquist plot in an Electrochemical Impedance Spectroscopy (Electrochemical Impedance Spectroscopy) by an Electrochemical Impedance Spectroscopy (Electrochemical Impedance Spectroscopy), and the results are shown in fig. 3 and 4. FIGS. 3a and 4a are actually measured electrochemical AC impedance data, and FIGS. 3b and 4b are Nyquist plots of AC impedance obtained by fitting the data of FIGS. 3a and 4a to ZView software. As can be seen from fig. 3 and 4, as the mass fraction of silver increases, the corrosion resistance of the silver-antimony alloy solid-state pH-responsive electrode increases (the larger the radius of the semicircle in the nyquist plot, the larger the representative polarization resistance, the better the corrosion resistance).
The invention discloses a silver-antimony alloy solid pH response electrode and a preparation method and application thereof, and a person skilled in the art can realize the solid pH response electrode by properly improving process parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the invention has been described in terms of preferred embodiments, it will be apparent to those skilled in the art that the technology can be practiced and applied by modifying or appropriately combining the products described herein without departing from the spirit and scope of the invention.
Claims (10)
1. The silver-antimony alloy solid pH response electrode is characterized by being made of a silver-antimony alloy material, wherein antimony accounts for wt% of the silver-antimony alloy material1% is: 27 percent to wt1Percent is less than 100 percent, and the mass of silver is hundredFraction wt2% is: 0 < wt2％≤73％。
2. The method for preparing silver-antimony alloy solid pH response electrode according to claim 1, wherein mass percent wt of antimony in silver-antimony alloy material1% is: 46 percent to wt1Percent is less than 100 percent, and the mass percent of silver is wt2% is: 0 < wt2％≤54％。
3. The method for preparing the silver-antimony alloy solid pH response electrode according to claim 1, wherein in the silver-antimony alloy material, the mass percent of antimony is 75%, and the mass percent of silver is 25%.
4. The method for preparing a silver-antimony alloy solid pH responsive electrode of claim 1, comprising the steps of:
step one, selecting silver powder and antimony powder as raw materials, weighing the silver powder and the antimony powder which meet the mass percentage, and grinding and mixing the silver powder and the antimony powder uniformly;
step two, preparing a silver-antimony alloy electrode bar;
and step three, grinding one end of the silver-antimony alloy electrode bar to be flat as a pH response surface, and welding the other end of the silver-antimony alloy electrode bar with a lead to prepare the silver-antimony alloy solid pH response electrode.
5. The method for preparing the silver-antimony alloy solid pH response electrode according to claim 4, wherein in the first step, the silver powder is high-purity silver powder, and the antimony powder is high-purity antimony powder.
6. The method for preparing silver-antimony alloy solid pH response electrode according to claim 4, characterized in that in the second step, a high temperature molten metal casting method is selected, a glass tube is used as a casting mold to prepare a silver-antimony alloy electrode bar, or a magnetron sputtering method is selected to prepare a silver-antimony alloy electrode film, or a high temperature chemical vapor deposition method is selected to prepare a silver-antimony alloy electrode film.
7. The method for preparing the silver-antimony alloy solid pH response electrode according to claim 4, wherein in the second step, the parameters of the high temperature molten metal casting method are as follows: the melting temperature is more than or equal to 670 ℃, the heat preservation time is 4-6h, and the silver-antimony alloy electrode rod is obtained after the furnace is naturally cooled to the room temperature.
8. The method for preparing silver-antimony alloy solid pH response electrode according to claim 7, wherein the melting temperature is 670 ℃ and the holding time is 5 h.
9. The use of the silver-antimony alloy solid pH-responsive electrode of claim 1 in the preparation of an all-solid composite pH sensor, wherein the all-solid composite pH sensor is made by compounding the silver-antimony alloy solid pH-responsive electrode with a reference electrode.
10. Use of a silver-antimony alloy solid state pH-responsive electrode according to claim 9, wherein the reference electrode is: a solid silver/silver chloride reference electrode, a saturated calomel reference electrode, or a mercury/mercury oxide reference electrode.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102565164A (en) * | 2012-02-01 | 2012-07-11 | 江苏大学 | Method for producing antimony pH electrode modified by two layers of films |
| CN106018516A (en) * | 2016-05-09 | 2016-10-12 | 江苏大学 | Method for preparing graphene modified composite slab pH sensor |
| CN109342520A (en) * | 2018-09-29 | 2019-02-15 | 中国科学院长春应用化学研究所 | A kind of all-solid-state pH combination electrode device and preparation method thereof |
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- 2020-09-09 CN CN202010941406.5A patent/CN112067677A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102565164A (en) * | 2012-02-01 | 2012-07-11 | 江苏大学 | Method for producing antimony pH electrode modified by two layers of films |
| CN106018516A (en) * | 2016-05-09 | 2016-10-12 | 江苏大学 | Method for preparing graphene modified composite slab pH sensor |
| CN109342520A (en) * | 2018-09-29 | 2019-02-15 | 中国科学院长春应用化学研究所 | A kind of all-solid-state pH combination electrode device and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| YAOSHENG LIU等: "Fabrication, improved performance, and response mechanism of binary Ag-Sb alloy pH electrodes", 《ELECTROCHIMICA ACTA》 * |
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Application publication date: 20201211 |