CN109557136B - Method for measuring ion concentration in electrolyte under high voltage - Google Patents
Method for measuring ion concentration in electrolyte under high voltage Download PDFInfo
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- CN109557136B CN109557136B CN201811218618.XA CN201811218618A CN109557136B CN 109557136 B CN109557136 B CN 109557136B CN 201811218618 A CN201811218618 A CN 201811218618A CN 109557136 B CN109557136 B CN 109557136B
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000012528 membrane Substances 0.000 claims abstract description 46
- 150000002500 ions Chemical class 0.000 claims abstract description 37
- 230000005540 biological transmission Effects 0.000 claims abstract description 30
- 238000012544 monitoring process Methods 0.000 claims abstract description 4
- 230000001105 regulatory effect Effects 0.000 claims abstract description 4
- 239000004020 conductor Substances 0.000 claims description 23
- 238000005259 measurement Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 3
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 claims description 3
- 230000005518 electrochemistry Effects 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 5
- 230000008054 signal transmission Effects 0.000 description 5
- 230000003321 amplification Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000003199 nucleic acid amplification method Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 230000003071 parasitic effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
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Abstract
The invention relates to the field of electrochemistry, in particular to a method for measuring ion concentration in electrolyte under high voltage, wherein an electrolyte sample to be measured is added into a sample tank, a corresponding membrane electrode is selected, and the membrane electrode, a reference electrode and a temperature sensor are all arranged in the electrolyte sample; starting a high-voltage direct-current power supply, and generating a voltage difference between the electrode I and the electrode II; regulating the air pressure inside the spark switch; adjusting the positions of the laser and the lens to enable laser pulses emitted by the laser to vertically irradiate to the top end of the electrode I through the lens, the window III and the through hole of the electrode II; monitoring a voltage waveform between electrode I and electrode II of the spark switch; adjusting the power and duration of laser pulses emitted by the laser to ensure that the gas between the electrode I and the electrode II is broken down, and conducting a spark switch; generating a voltage difference between the core wire of the transmission line II and the sample tank shell, and applying the voltage difference to the electrolyte sample; the voltage signals of the membrane electrode and the reference electrode are amplified and processed and then output; analyzing to obtain the concentration value of the ions to be detected.
Description
Technical Field
The invention relates to the field of electrochemistry, in particular to a method for measuring the concentration of ions in electrolyte under high voltage, which can be used for measuring the concentration of lower ions in the electrolyte under high voltage.
Background
The electrolyte is widely used in the chemical industry field such as batteries and capacitors, and is also largely involved in the biological field, and the research on the electrolyte comprises the research on the ion concentration and the characteristics of the electrolyte under high voltage, namely, the defect one in the prior art: in the prior art, an acidometer is generally used for measuring the ion concentration, and the lower measurement limit of the acidometer is only 10 -4 Molar/liter orders; the defects of the prior art are as follows: when the characteristics of the electrolyte under the high voltage condition are studied, a voltage square wave pulse with a certain duration and amplitude needs to be applied to the electrolyte, the duration and the amplitude of the voltage square wave pulse need to be adjustable, a spark switch is generally adopted in the prior art to adjust the amplitude of the voltage pulse by adjusting the distance between an anode and a cathode of the spark switch and the air pressure, but the rising time and the amplitude of the voltage pulse generated by the method can generate a certain jitter to influence the stability of the voltage pulse, and the method for measuring the ion concentration in the electrolyte under the high voltage can solve the problem.
Disclosure of Invention
In order to solve the problems, the method adopts a method that laser is perpendicularly incident to the cathode surface to trigger a spark switch to generate voltage pulses, and applies stable and controllable high-voltage square wave pulses to electrolyte, and in addition, adopts a specially designed potential measuring circuit to measure the ion concentration in the electrolyte.
The technical scheme adopted by the invention is as follows:
the ion concentration measuring device in the electrolyte under high voltage comprises a high-voltage direct current power supply, a charging resistor, a charging wire, a spark switch, a lens, a laser power supply, a pulse generator, a power distributor, an attenuator, a transmission line I, an impedance matching circuit, an oscilloscope, a transmission line II, a sample tank and a potential measuring circuit, wherein the high voltage is in a range of 5kV to 15kV, and the power distributor is provided with an input end, an output end I and an output end II; the spark switch comprises a shell, an electrode I, a vent, a window I, an electrode II, a window II, an insulating bottom cover and a window III; the high-voltage direct current power supply, the charging resistor, the charging wire and an electrode II of the spark switch are sequentially connected in a cable manner, an electrode I of the spark switch is connected with an input end of the power distributor, an output end I of the power distributor is sequentially connected with a transmission line II and a sample groove in a cable manner, a core wire of the transmission line II is insulated from a shell of the sample groove, the shell of the sample groove is grounded, an output end II of the power distributor is sequentially connected with an attenuator, a transmission line I, an impedance matching circuit and an oscilloscope in a cable manner, the laser power supply and the pulse generator are sequentially connected in a cable manner, the lens is positioned between the spark switch and the laser, and laser emitted by the laser can be emitted into the spark switch through the lens; the shell of the spark switch is cylindrical, an insulating bottom cover is connected below the shell, an electrode I is arranged above the inside of the shell, the top end of the electrode I is downward and hemispherical, an electrode II is arranged on the insulating bottom cover, the top end of the electrode II is upward and hemispherical, a window III is arranged at the lower end of the electrode II, the electrode II is provided with a through hole along an axis, laser emitted by a laser can sequentially pass through the window III and the through hole and then shoot at the top end of the electrode I, the distance between the top end of the electrode I and the top end of the electrode II can be adjusted, a vent, the window I and the window II are arranged on the side surface of the shell, the laser emitted by the laser can be shot at the top end of the electrode I through the window II by adjusting the position of the spark switch, and the vent can be used for carrying out inflation and deflation operation on the spark switch so as to control the air pressure inside the spark switch, and the window I is used for observing the spot size of the laser emitted by the laser to the top end of the electrode I; the potential measurement circuit comprises a membrane electrode, a reference electrode, a temperature sensor, a central conductor, a shielding layer, a grounding layer, an operational amplifier, a buffer, a filter I, a filter II, a digital converter I, a digital converter II, a microcontroller, a direct current power supply I, a direct current power supply II, a USB converter and a connector, wherein the membrane electrode, the reference electrode and the temperature sensor are all positioned in a sample tank, the operational amplifier is provided with a same-direction input end, a reverse input end and an output end, the buffer is provided with an input end and an output end, the periphery of the central conductor is sequentially provided with the shielding layer and the grounding layer, the membrane electrode is connected with the same-direction input end of the operational amplifier through the central conductor, the reference electrode is connected with the reverse input end of the operational amplifier through the grounding layer, the output end of the operational amplifier is connected with the input end of the buffer, the output end of the buffer is connected with the shielding layer, the output end of the operational amplifier is sequentially connected with the filter I, the digital converter I and the microcontroller, the temperature sensor is sequentially connected with the filter II, the digital converter II and the microcontroller, the USB converter and the microcontroller are sequentially connected with the connector, and the direct current power supply I and the microcontroller are respectively connected with the connector; electrode I and electrode II were each in a ratio of 6:4, the electrode I is made of tungsten copper alloy, the hemispherical diameter of the top end of the electrode I is 3 mm, the hemispherical diameter of the top end of the electrode II is 4 mm, and the adjusting range of the distance between the top end of the electrode I and the top end of the electrode II is 1 mm to 15 mm; the energy of each laser pulse emitted by the laser ranges from 200mJ to 900mJ, and the duration of each laser pulse ranges from 2 nanoseconds to 8 nanoseconds; the air pressure inside the spark switch ranges from 50kPa to 700kPa.
The potential measuring circuit works in the following manner:
the membrane electrode, the reference electrode and the temperature sensor are all positioned in electrolyte in the sample tank, and the membrane electrode has ion selectivity, and when the membrane electrode contacts with a solution containing ions to be detected, membrane potential directly related to the activity of the ions to be detected is generated at the interface of a sensitive membrane and the solution, namely, the membrane electrode has selective response to specific ions.
The coaxial signal transmission structure is formed by the central conductor, the shielding layer and the grounding layer and is used for connecting the membrane electrode, the reference electrode and the operational amplifier, wherein the central conductor is used for signal transmission, the shielding layer is used for shielding signals in the central conductor, and the grounding layer is grounded to prevent electromagnetic interference of the external environment. The operational amplifier and the buffer have a cut-off frequency of 3kHz at 3dB for amplifying analog signals generated by the membrane electrode and outputting a direct current voltage, and in addition, the operational amplifier and the buffer can prevent electromagnetic interference and parasitic currents between the circuit and the environment. The filter I and the filter II are second-order Butterworth low-pass filters and are used for reducing 60Hz and frequency multiplication noise in the circuit. The digital converter I and the digital converter II respectively convert the analog signals output by the filter I and the filter II into digital signals, and the microcontroller is used for processing and storing the digital signals.
The analog signals generated by the membrane electrode and the reference electrode are transmitted to an operational amplifier which has a high input impedance, the direct current voltage drop over the transmission cable in the circuit will seriously affect the analog signals at the output of the operational amplifier, in order to minimize said voltage drop, a filter I is connected between the shielding layer and the ground layer, which is very sensitive to high frequency electromagnetic interference, since the operational amplifier has a high input impedance, and the output of the operational amplifier is connected with a filter I, which minimizes the voltage drop over the transmission cable in the circuit to a microvolts level.
The analog signals generated by the membrane electrode are amplified and filtered and then are converted into digital signals by the digital converter I and are transmitted to the microcontroller, the analog signals generated by the temperature sensor are filtered by the filter II and are then converted into digital signals by the digital converter II and are transmitted to the microcontroller, the microcontroller transmits the signals to the USB converter after processing and are transmitted to the connector, finally, the direct current power supply I outputs signals generated by the membrane electrode after amplification, the direct current power supply II outputs signals generated by the temperature sensor after amplification, the concentration information of ions to be detected in the electrolyte can be obtained by analyzing the voltage signals output by the direct current power supply I, and the temperature value in the electrolyte can be obtained by analyzing the voltage signals output by the direct current power supply II.
Square wave voltage pulse generation:
the electrode I is grounded, a high-voltage direct-current power supply applies voltage to the electrode II through a charging resistor and a charging wire, so that a high voltage difference exists in an area between the electrode II and the electrode I, laser emitted by the laser vertically irradiates the top end of the electrode I through a lens, a window III and a through hole of the electrode II, seed electrons are generated by the electrode I due to a photoelectric effect, the gas in the area between the electrode II and the electrode I is broken down by the high voltage, and a spark switch is conducted.
The advantage that laser vertically irradiates the top end of the electrode I through the lens, the window III and the through hole of the electrode II is that: compared with the condition that laser is obliquely incident on the top end of the electrode I, the delay time and jitter of the generated voltage pulse are much smaller depending on other experimental conditions, such as air pressure, air type, electrode material and electrode top end shape, and the voltage pulse is easier to control.
The method for measuring the ion concentration in the electrolyte under the high voltage adopts the ion concentration measuring device in the electrolyte under the high voltage, and comprises the following steps:
step 1, adding an electrolyte sample to be detected into a sample tank, selecting a corresponding membrane electrode according to the ion type to be detected in the electrolyte, and placing the membrane electrode, a reference electrode and a temperature sensor into the electrolyte sample;
step 2, turning on a high-voltage direct-current power supply to generate a voltage difference between the electrode I and the electrode II;
step 3, regulating the air pressure in the spark switch through the air vent, wherein the typical value of the air pressure is 300kPa;
step 4, turning on a laser power supply and a pulse generator, and adjusting the positions of the laser and the lens so that laser pulses emitted by the laser vertically irradiate to the top end of the electrode I through the lens, the window III and the through hole of the electrode II;
step 5, monitoring the voltage waveform between the electrode I and the electrode II of the spark switch through an oscilloscope;
step 6, adjusting the power and duration of laser pulse emitted by the laser through a laser power supply and a pulse generator, wherein the typical value of the pulse power is 400mJ, and the typical value of the pulse duration is 4 nanoseconds, so that the gas between the electrode I and the electrode II is broken down, and a spark switch is conducted;
step 7, generating a voltage difference between the core wire of the transmission line II and the sample tank shell in the on time of the spark switch, and applying the voltage difference to the electrolyte sample;
step 8, the voltage signals of the membrane electrode and the reference electrode are amplified and processed and then output through a direct current power supply I;
and 9, analyzing a voltage signal output by the direct current power supply I to obtain the concentration value of ions to be detected in the electrolyte.
The beneficial effects of the invention are as follows:
the method can apply stable and controllable high-voltage square wave pulse to the electrolyte, can measure the ion concentration in the electrolyte, and has low measurement lower limit.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic illustration of the present invention;
FIG. 2 is an enlarged schematic diagram of a spark switch;
fig. 3 is a schematic diagram of a potential measurement circuit.
In the figure, 1. High voltage DC power supply, 2. Charging resistor, 3. Charging wire, 4. Spark switch, 4-1. Housing, 4-2. Electrode I,4-3. Vent, 4-4. Window I,4-5. Electrode II,4-6. Window II,4-7. Insulating bottom cover, 4-8. Window III,5. Lens, 6. Laser, 7. Laser power supply, 8. Pulse generator, 9. Power splitter, 10. Attenuator, 11. Transmission line I,12. Impedance matching circuit, 13. Oscilloscope, 14. Transmission line II,15. Sample cell, 16. Potential measuring circuit, 16-1. Membrane electrode, 16-2. Reference electrode, 16-3. Temperature sensor, 16-4. Center conductor, 16-5. Shielding layer, 16-6. Ground plane, 16-7. Operational amplifier, 16-8. Buffer, 16-9. Filter I,16-10. Filter II,16-11. Digitizer I,16-12. DC power supply, 16-16. DC power supply, 16-16. DC power supply, 16.
Detailed Description
Fig. 1 is a schematic diagram of the invention, xyz is a three-dimensional space coordinate system, fig. 2 is an enlarged schematic diagram of a spark switch,
the ion concentration measuring device in the electrolyte under high voltage comprises a high-voltage direct current power supply (1), a charging resistor (2), a charging wire (3), a spark switch (4), a lens (5), a laser (6), a laser power supply (7), a pulse generator (8), a power distributor (9), an attenuator (10), a transmission line I (11), an impedance matching circuit (12), an oscilloscope (13), a transmission line II (14), a sample tank (15) and a potential measuring circuit (16), wherein the high voltage range is 5kV to 15kV, and the power distributor (9) is provided with an input end, an output end I and an output end II; the spark switch (4) comprises a shell (4-1), an electrode I (4-2), a vent (4-3), a window I (4-4), an electrode II (4-5), a window II (4-6), an insulating bottom cover (4-7) and a window III (4-8); the high-voltage direct current power supply (1), the charging resistor (2), the charging wire (3) and an electrode II (4-5) of the spark switch (4) are sequentially connected in a cable mode, an electrode I (4-2) of the spark switch (4) is connected with an input end of the power distributor (9), an output end I of the power distributor (9) is sequentially connected with a transmission wire II (14) and a sample groove (15) in a cable mode, a core wire of the transmission wire II (14) is insulated with a shell of the sample groove (15), the shell of the sample groove (15) is grounded, an output end II of the power distributor (9) is sequentially connected with an attenuator (10), a transmission wire I (11), an impedance matching circuit (12) and an oscilloscope (13) in a cable mode, a laser (6), a laser power supply (7) and a pulse generator (8) are sequentially connected in a cable mode, the lens (5) is located between the spark switch (4) and the laser (6), and laser emitted by the laser (6) can enter the spark switch (4) through the lens (5); the shell (4-1) of the spark switch (4) is cylindrical, an insulating bottom cover (4-7) is connected below, an electrode I (4-2) is installed above the inside of the shell (4-1), the top end of the electrode I (4-2) is downward and hemispherical, an electrode II (4-5) is installed on the insulating bottom cover (4-7), the top end of the electrode II (4-5) is upward and hemispherical, a window III (4-8) is installed at the lower end of the electrode II (4-5), the electrode II (4-5) is provided with a through hole along an axis, laser emitted by a laser (6) can sequentially pass through the window III (4-8) and the through hole, the distance between the top end of the electrode I (4-2) and the top end of the electrode II (4-5) can be adjusted, the adjusting range is 1 millimeter to 15 millimeters, and both the electrode I (4-2) and the electrode II (4-5) are in proportion of 6:4, wherein the side surface of the shell (4-1) is provided with a vent (4-3), a window I (4-4) and a window II (4-6), the position of the spark switch (4) is adjusted, so that laser emitted by the laser (6) can be emitted to the top end of the electrode I (4-2) through the window II (4-6), the vent (4-3) can be used for carrying out air charging and air discharging operation on the spark switch (4) to control the air pressure in the spark switch (4), the air pressure ranges from 50kPa to 700kPa, and the window I (4-4) is used for observing the spot size of the laser emitted by the laser (6) to the top end of the electrode I (4-2); the top hemispherical diameter of electrode I (4-2) is 3 mm, and the top hemispherical diameter of electrode II (4-5) is 4 mm; the energy of each laser pulse emitted by the laser (6) ranges from 200mJ to 900mJ, and the duration of each laser pulse ranges from 2 nanoseconds to 8 nanoseconds.
As shown in fig. 3, which is a schematic diagram of a potential measuring circuit, the potential measuring circuit (16) comprises a membrane electrode (16-1), a reference electrode (16-2), a temperature sensor (16-3), a central conductor (16-4), a shielding layer (16-5), a ground layer (16-6), an operational amplifier (16-7), a buffer (16-8), a filter I (16-9), a filter II (16-10), a digital converter I (16-11), a digital converter II (16-12), a microcontroller (16-13), a direct current power supply I (16-14), a direct current power supply II (16-15), a USB converter (16-16) and a connector (16-17), wherein the membrane electrode (16-1), the reference electrode (16-2) and the temperature sensor (16-3) are all positioned in a sample tank (15), the operational amplifier (16-7) has a same-directional input end, a reverse input end and an output end, the buffer (16-8) has an input end and an output end, the periphery of the central conductor (16-4) has the shielding layer (16-6) and the ground layer (16-6) in sequence, the membrane electrode (16-1) is connected with the same-direction input end of the operational amplifier (16-7) through the central conductor (16-4), the reference electrode (16-2) is connected with the reverse input end of the operational amplifier (16-7) through the ground layer (16-6), the output end of the operational amplifier (16-7) is connected with the input end of the buffer (16-8), the output end of the buffer (16-8) is connected with the shielding layer (16-5), the output end of the operational amplifier (16-7) is sequentially connected with the filter I (16-9), the digital converter I (16-11) and the microcontroller (16-13), the temperature sensor (16-3) is sequentially connected with the filter II (16-10), the digital converter II (16-12) and the microcontroller (16-13), the microcontroller (16-13) is sequentially connected with the USB converter (16-16) and the connector (16-17), and the direct current power supply I (16-14) and the direct current power supply II (16-15) are respectively connected with the connector (16-17).
The potential measuring circuit (16) operates in the following manner:
the membrane electrode (16-1), the reference electrode (16-2) and the temperature sensor (16-3) are all positioned in the electrolyte in the sample tank (15), the membrane electrode (16-1) has ion selectivity, and when the membrane electrode is contacted with a solution containing ions to be detected, a membrane potential directly related to the activity of the ions to be detected is generated at the interface of a sensitive membrane and the solution, namely, the membrane electrode has selective response to specific ions.
The central conductor (16-4), the shielding layer (16-5) and the grounding layer (16-6) form a coaxial signal transmission structure, and the coaxial signal transmission structure is used for connecting the membrane electrode (16-1), the reference electrode (16-2) and the operational amplifier (16-7), wherein the central conductor (16-4) is used for signal transmission, the shielding layer (16-5) is used for shielding signals in the central conductor (16-4), and the grounding layer (16-6) is grounded to prevent electromagnetic interference of the external environment. The operational amplifier (16-7) and the buffer (16-8) have a cut-off frequency of 3kHz at 3dB for amplifying the analog signal generated by the membrane electrode (16-1) and outputting a DC voltage, and the operational amplifier (16-7) and the buffer (16-8) can prevent electromagnetic interference and parasitic current between the circuit and the environment. The filter I (16-9) and the filter II (16-10) are second-order Butterworth low-pass filters for reducing 60Hz and frequency multiplication noise in the circuit. The digital converter I (16-11) and the digital converter II (16-12) respectively convert the analog signals output by the filter I (16-9) and the filter II (16-10) into digital signals, and the microcontroller (16-13) is used for processing and storing the digital signals.
The analog signals generated by the membrane electrode (16-1) and the reference electrode (16-2) are transmitted to the operational amplifier (16-7), the operational amplifier (16-7) has high input impedance, and since the impedance of the membrane electrode (16-1) and the reference electrode (16-2) is in the order of hundreds of megaohms, the direct current voltage drop on the transmission cable in the circuit can seriously affect the analog signals at the output end of the operational amplifier (16-7), in order to minimize the voltage drop, the filter I (16-9) is connected between the shielding layer (16-5) and the ground layer (16-6), and since the operational amplifier (16-7) has high input impedance, the operational amplifier (16-7) is very sensitive to high frequency electromagnetic interference, and the filter I (16-9) is connected with the output end of the operational amplifier (16-7), so that the voltage drop on the transmission cable in the circuit is minimized to the microvoltage level.
The analog signals generated by the membrane electrode (16-1) are amplified and filtered, then are converted into digital signals by the digital converter I (16-11) and are transmitted to the microcontroller (16-13), the analog signals generated by the temperature sensor (16-3) are filtered by the filter II (16-10), then are converted into digital signals by the digital converter II (16-12) and are transmitted to the microcontroller (16-13), the microcontroller (16-13) processes the signals and transmits the digital signals to the USB converter (16-16) and is transmitted to the connector (16-17), finally, the direct current power supply I (16-14) outputs the signals generated by the membrane electrode (16-1) after the amplification process, the direct current power supply II (16-15) outputs the signals generated by the temperature sensor (16-3) after the amplification process, the voltage signals output by the direct current power supply I (16-14) are analyzed, so that the concentration information of ions to be detected in the electrolyte can be obtained, and the voltage signals output by the direct current power supply II (16-15) are analyzed, so that the temperature value in the electrolyte can be obtained.
Square wave voltage pulse generation:
the electrode I (4-2) is grounded, the high-voltage direct current power supply (1) applies voltage to the electrode II (4-5) through the charging resistor (2) and the charging wire (3), so that a high voltage difference exists in the area between the electrode II (4-5) and the electrode I (4-2), laser emitted by the laser (6) vertically irradiates the top end of the electrode I (4-2) through the lens (5), the window III (4-8) and the through hole of the electrode II (4-5), seed electrons are generated by the electrode I (4-2) due to the photoelectric effect, and the gas in the area between the electrode II (4-5) and the electrode I (4-2) is broken down by the high voltage, so that the spark switch (4) is conducted.
The advantage of laser perpendicularly penetrating the through hole of the lens (5), the window III (4-8) and the electrode II (4-5) to the top end of the electrode I (4-2) is that: compared with the case that the laser is obliquely incident on the top end of the electrode I (4-2), the delay time and jitter of the generated voltage pulse are much smaller, and the voltage pulse is easier to control due to the fact that the experimental conditions such as air pressure, air type, electrode material and electrode top end shape are much less dependent.
The ion concentration measuring device in the electrolyte under high voltage comprises a high-voltage direct current power supply (1), a charging resistor (2), a charging wire (3), a spark switch (4), a lens (5), a laser (6), a laser power supply (7), a pulse generator (8), a power distributor (9), an attenuator (10), a transmission line I (11), an impedance matching circuit (12), an oscilloscope (13), a transmission line II (14), a sample tank (15) and a potential measuring circuit (16), wherein the high voltage range is 5kV to 15kV, and the power distributor (9) is provided with an input end, an output end I and an output end II; the spark switch (4) comprises a shell (4-1), an electrode I (4-2), a vent (4-3), a window I (4-4), an electrode II (4-5), a window II (4-6), an insulating bottom cover (4-7) and a window III (4-8); the high-voltage direct current power supply (1), the charging resistor (2), the charging wire (3) and an electrode II (4-5) of the spark switch (4) are sequentially connected in a cable mode, an electrode I (4-2) of the spark switch (4) is connected with an input end of the power distributor (9), an output end I of the power distributor (9) is sequentially connected with a transmission wire II (14) and a sample groove (15) in a cable mode, a core wire of the transmission wire II (14) is insulated with a shell of the sample groove (15), the shell of the sample groove (15) is grounded, an output end II of the power distributor (9) is sequentially connected with an attenuator (10), a transmission wire I (11), an impedance matching circuit (12) and an oscilloscope (13) in a cable mode, a laser (6), a laser power supply (7) and a pulse generator (8) are sequentially connected in a cable mode, the lens (5) is located between the spark switch (4) and the laser (6), and laser emitted by the laser (6) can enter the spark switch (4) through the lens (5); the shell (4-1) of the spark switch (4) is cylindrical, an insulating bottom cover (4-7) is connected below the shell (4-1), an electrode I (4-2) is arranged above the inside of the shell (4-1), the top end of the electrode I (4-2) is downward and hemispherical, the electrode II (4-5) is arranged above the insulating bottom cover (4-7), the top end of the electrode II (4-5) is upward and hemispherical, a window III (4-8) is arranged at the lower end of the electrode II (4-5), the electrode II (4-5) is provided with a through hole along the axis, laser emitted by the laser (6) can sequentially pass through the window III (4-8) and the through hole, the distance between the top end of the electrode I (4-2) and the top end of the electrode II (4-5) can be adjusted, the side surface of the shell (4-1) is provided with a vent (4-3), the window I (4-4) and the window II (4-6), the position of the switch (4) is adjusted, the laser emitted by the laser (6) to the electrode I (4-6), the air-filling and air-discharging operation of the spark switch (4) can be carried out through the air-filling and air-discharging operation of the spark switch (4), and the window I (4-4) is used for observing the spot size of laser emitted by the laser (6) to the top end of the electrode I (4-2); the potential measurement circuit (16) comprises a membrane electrode (16-1), a reference electrode (16-2), a temperature sensor (16-3), a central conductor (16-4), a shielding layer (16-5), a ground layer (16-6), an operational amplifier (16-7), a buffer (16-8), a filter I (16-9), a filter II (16-10), a digital converter I (16-11), a digital converter II (16-12), a microcontroller (16-13), a direct current power supply I (16-14), a direct current power supply II (16-15), a USB converter (16-16) and a connector (16-17), wherein the membrane electrode (16-1), the reference electrode (16-2) and the temperature sensor (16-3) are all positioned in a sample tank (15), the operational amplifier (16-7) is provided with a homodromous input end, a reverse input end and an output end, the buffer (16-8) is provided with an input end and an output end, the periphery of the central conductor (16-4) is sequentially provided with the shielding layer (16-5) and the ground layer (16-6) and the central conductor (16-6) which are connected with the central conductor (16-4) through the central conductor (16-1), the reference electrode (16-2) is connected with the reverse input end of the operational amplifier (16-7) through the grounding layer (16-6), the output end of the operational amplifier (16-7) is connected with the input end of the buffer (16-8), the output end of the buffer (16-8) is connected with the shielding layer (16-5), the output end of the operational amplifier (16-7) is sequentially connected with the filter I (16-9), the digital converter I (16-11) and the microcontroller (16-13), the temperature sensor (16-3) is sequentially connected with the filter II (16-10), the digital converter II (16-12) and the microcontroller (16-13), the microcontroller (16-13) is sequentially connected with the USB converter (16-16) and the connector (16-17), and the direct current power supply I (16-14) and the direct current power supply II (16-15) are respectively connected with the connector (16-17); the electrode I (4-2) and the electrode II (4-5) are both made of tungsten copper alloy with the ratio of 6:4, the hemispherical diameter of the top end of the electrode I (4-2) is 3 mm, the hemispherical diameter of the top end of the electrode II (4-5) is 4 mm, and the adjustment range of the distance between the top end of the electrode I (4-2) and the top end of the electrode II (4-5) is 1 mm to 15 mm; the energy of each laser pulse emitted by the laser (6) ranges from 200mJ to 900mJ, and the duration of each laser pulse ranges from 2 nanoseconds to 8 nanoseconds; the air pressure inside the spark switch (4) ranges from 50kPa to 700kPa.
The method for measuring the ion concentration in the electrolyte under the high voltage adopts the ion concentration measuring device in the electrolyte under the high voltage, and comprises the following steps:
step 1, adding an electrolyte sample to be detected into a sample tank (15), selecting a corresponding membrane electrode (16-1) according to the ion type to be detected in the electrolyte, and placing the membrane electrode (16-1), a reference electrode (16-2) and a temperature sensor (16-3) into the electrolyte sample;
step 2, starting a high-voltage direct current power supply (1) to generate a voltage difference between an electrode I (4-2) and an electrode II (4-5);
step 3, regulating the air pressure in the spark switch (4) through the air port (4-3), wherein the typical value of the air pressure is 300kPa;
step 4, a laser power supply (7) and a pulse generator (8) are started, and the positions of a laser (6) and a lens (5) are adjusted, so that laser pulses emitted by the laser (6) vertically irradiate to the top end of an electrode I (4-2) through holes of the lens (5), a window III (4-8) and an electrode II (4-5);
step 5, monitoring the voltage waveform between the electrode I (4-2) and the electrode II (4-5) of the spark switch (4) through an oscilloscope (13);
step 6, adjusting the power and duration of laser pulses emitted by the laser (6) through a laser power supply (7) and a pulse generator (8), wherein the typical pulse power value is 400mJ, and the typical pulse duration value is 4 nanoseconds, so that the gas between the electrode I (4-2) and the electrode II (4-5) is broken down, and the spark switch (4) is turned on;
step 7, generating a voltage difference between the core wire of the transmission line II (14) and the shell of the sample tank (15) in the on time of the spark switch (4), and applying the voltage difference to the electrolyte sample;
step 8, the voltage signals of the membrane electrode (16-1) and the reference electrode (16-2) are amplified and processed and then output through a direct current power supply I (16-14);
and 9, analyzing the voltage signal output by the direct current power supply I (16-14) to obtain the concentration value of ions to be detected in the electrolyte.
The invention adopts a method that laser pulse is vertically incident to the cathode surface to trigger the spark switch to generate stable and controllable high-voltage square wave pulse to be applied to electrolyte, and adopts a specially designed potential measuring circuit to measure the ion concentration in the electrolyte, thus having high measuring sensitivity.
Claims (1)
1. The method for measuring the ion concentration in the electrolyte under high voltage comprises a high-voltage direct current power supply (1), a charging resistor (2), a charging wire (3), a spark switch (4), a lens (5), a laser (6), a laser power supply (7), a pulse generator (8), a power distributor (9), an attenuator (10), a transmission line I (11), an impedance matching circuit (12), an oscilloscope (13), a transmission line II (14), a sample tank (15) and a potential measuring circuit (16), wherein the high voltage range is 5kV to 15kV, and the power distributor (9) is provided with an input end, an output end I and an output end II; the spark switch (4) comprises a shell (4-1), an electrode I (4-2), a vent (4-3), a window I (4-4), an electrode II (4-5), a window II (4-6), an insulating bottom cover (4-7) and a window III (4-8); the high-voltage direct current power supply (1), the charging resistor (2), the charging wire (3) and an electrode II (4-5) of the spark switch (4) are sequentially connected in a cable mode, an electrode I (4-2) of the spark switch (4) is connected with an input end of the power distributor (9), an output end I of the power distributor (9) is sequentially connected with a transmission wire II (14) and a sample groove (15) in a cable mode, a core wire of the transmission wire II (14) is insulated with a shell of the sample groove (15), the shell of the sample groove (15) is grounded, an output end II of the power distributor (9) is sequentially connected with an attenuator (10), a transmission wire I (11), an impedance matching circuit (12) and an oscilloscope (13) in a cable mode, a laser (6), a laser power supply (7) and a pulse generator (8) are sequentially connected in a cable mode, the lens (5) is located between the spark switch (4) and the laser (6), and laser emitted by the laser (6) can enter the spark switch (4) through the lens (5); the shell (4-1) of the spark switch (4) is cylindrical, an insulating bottom cover (4-7) is connected below the shell (4-1), an electrode I (4-2) is arranged above the inside of the shell (4-1), the top end of the electrode I (4-2) is downward and hemispherical, the electrode II (4-5) is arranged above the insulating bottom cover (4-7), the top end of the electrode II (4-5) is upward and hemispherical, a window III (4-8) is arranged at the lower end of the electrode II (4-5), the electrode II (4-5) is provided with a through hole along the axis, laser emitted by the laser (6) can sequentially pass through the window III (4-8) and the through hole, the distance between the top end of the electrode I (4-2) and the top end of the electrode II (4-5) can be adjusted, the side surface of the shell (4-1) is provided with a vent (4-3), the window I (4-4) and the window II (4-6), the position of the switch (4) is adjusted, the laser emitted by the laser (6) to the electrode I (4-6), the air-filling and air-discharging operation of the spark switch (4) can be carried out through the air-filling and air-discharging operation of the spark switch (4), and the window I (4-4) is used for observing the spot size of laser emitted by the laser (6) to the top end of the electrode I (4-2); the potential measurement circuit (16) comprises a membrane electrode (16-1), a reference electrode (16-2), a temperature sensor (16-3), a central conductor (16-4), a shielding layer (16-5), a ground layer (16-6), an operational amplifier (16-7), a buffer (16-8), a filter I (16-9), a filter II (16-10), a digital converter I (16-11), a digital converter II (16-12), a microcontroller (16-13), a direct current power supply I (16-14), a direct current power supply II (16-15), a USB converter (16-16) and a connector (16-17), wherein the membrane electrode (16-1), the reference electrode (16-2) and the temperature sensor (16-3) are all positioned in a sample tank (15), the operational amplifier (16-7) is provided with a homodromous input end, a reverse input end and an output end, the buffer (16-8) is provided with an input end and an output end, the periphery of the central conductor (16-4) is sequentially provided with the shielding layer (16-5) and the ground layer (16-6) and the central conductor (16-6) which are connected with the central conductor (16-4) through the central conductor (16-1), the reference electrode (16-2) is connected with the reverse input end of the operational amplifier (16-7) through the grounding layer (16-6), the output end of the operational amplifier (16-7) is connected with the input end of the buffer (16-8), the output end of the buffer (16-8) is connected with the shielding layer (16-5), the output end of the operational amplifier (16-7) is sequentially connected with the filter I (16-9), the digital converter I (16-11) and the microcontroller (16-13), the temperature sensor (16-3) is sequentially connected with the filter II (16-10), the digital converter II (16-12) and the microcontroller (16-13), the microcontroller (16-13) is sequentially connected with the USB converter (16-16) and the connector (16-17), and the direct current power supply I (16-14) and the direct current power supply 1I (16-15) are respectively connected with the connector (16-17); the electrode I (4-2) and the electrode II (4-5) are both made of tungsten copper alloy with the ratio of 6:4, the hemispherical diameter of the top end of the electrode I (4-2) is 3 mm, the hemispherical diameter of the top end of the electrode II (4-5) is 4 mm, and the adjustment range of the distance between the top end of the electrode I (4-2) and the top end of the electrode II (4-5) is 1 mm to 15 mm; the energy of each laser pulse emitted by the laser (6) ranges from 200mJ to 900mJ, and the duration of each laser pulse ranges from 2 nanoseconds to 8 nanoseconds; the air pressure inside the spark switch (4) ranges from 50kPa to 700kPa,
the method is characterized in that: the method for measuring the ion concentration in the electrolyte under the high voltage adopts the ion concentration measuring device in the electrolyte under the high voltage, and comprises the following steps:
step 1, adding an electrolyte sample to be detected into a sample tank (15), selecting a corresponding membrane electrode (16-1) according to the ion type to be detected in the electrolyte, and placing the membrane electrode (16-1), a reference electrode (16-2) and a temperature sensor (16-3) into the electrolyte sample;
step 2, starting a high-voltage direct current power supply (1) to generate a voltage difference between an electrode I (4-2) and an electrode II (4-5);
step 3, regulating the air pressure in the spark switch (4) through the air port (4-3), wherein the typical value of the air pressure is 300kPa;
step 4, a laser power supply (7) and a pulse generator (8) are started, and the positions of a laser (6) and a lens (5) are adjusted, so that laser pulses emitted by the laser (6) vertically irradiate to the top end of an electrode I (4-2) through holes of the lens (5), a window III (4-8) and an electrode II (4-5);
step 5, monitoring the voltage waveform between the electrode I (4-2) and the electrode II (4-5) of the spark switch (4) through an oscilloscope (13);
step 6, adjusting the power and duration of laser pulses emitted by the laser (6) through a laser power supply (7) and a pulse generator (8), wherein the typical pulse power value is 400mJ, and the typical pulse duration value is 4 nanoseconds, so that the gas between the electrode I (4-2) and the electrode II (4-5) is broken down, and the spark switch (4) is turned on;
step 7, generating a voltage difference between the core wire of the transmission line II (14) and the shell of the sample tank (15) in the on time of the spark switch (4), and applying the voltage difference to the electrolyte sample;
step 8, the voltage signals of the membrane electrode (16-1) and the reference electrode (16-2) are amplified and processed and then output through a direct current power supply I (16-14);
and 9, analyzing the voltage signal output by the direct current power supply I (16-14) to obtain the concentration value of ions to be detected in the electrolyte.
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