CN107688048B - Reverse-addition type potentiostat and IV conversion measurement circuit for electrochemical measurement - Google Patents
Reverse-addition type potentiostat and IV conversion measurement circuit for electrochemical measurement Download PDFInfo
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Abstract
The invention provides a reverse addition type potentiostat and an IV conversion measurement circuit which can be used for electrochemical measurement, comprising the following components: the device comprises a potentiostat, an IV conversion circuit and an electrolytic cell, wherein the positive input end of the potentiostat is connected with a function generator, the reverse input and output ends of the potentiostat are connected with the electrolytic cell, so that a closed loop of negative feedback amplification is formed by the potentiostat and the electrolytic cell, and polarized current is output; the negative input end of the IV conversion circuit is connected with the electrolytic cell, the positive input end of the IV conversion circuit is grounded, and the output end of the IV conversion circuit is connected with a subsequent receiving signal acquisition loop and is used for converting polarized current output by the electrolytic cell in the electrochemical reaction process into a voltage signal for data acquisition and processing by the subsequent receiving signal acquisition loop. The invention has higher stability and conversion precision under high-speed control voltage; the current measurement resolution is high and the repeatability is good.
Description
Technical Field
The invention relates to the technical field of potentiostat, in particular to a high-precision reverse addition potentiostat capable of being used for electrochemical measurement and an IV conversion measurement circuit.
Background
The existing constant potentiometer circuit has the problems of poor stability, low conversion precision and resolution, poor repeatability, weak anti-interference capability and the like.
Disclosure of Invention
The object of the present invention is to solve at least one of the technical drawbacks.
Therefore, the invention aims to provide a reverse addition type potentiostat and an IV conversion measurement circuit which can be used for electrochemical measurement.
In order to achieve the above object, an embodiment of the present invention provides a reverse-additive potentiostat and an IV-conversion measurement circuit, including: a potentiostat, an IV conversion circuit and an electrolytic cell, wherein,
The positive input end of the potentiostat is connected with the function generator, and the reverse input and output ends of the potentiostat are connected with the electrolytic cell to form a closed loop of negative feedback amplification by the potentiostat and the electrolytic cell and output polarized current;
The negative input end of the IV conversion circuit is connected with the electrolytic cell, the positive input end of the IV conversion circuit is connected with the ground, and the output end of the IV conversion circuit is connected with a subsequent receiving signal acquisition loop and is used for converting polarized current output by the electrolytic cell in the electrochemical reaction process into a voltage signal for data acquisition and processing by the subsequent receiving signal acquisition loop.
Further, the potentiostat and the IV conversion circuit both employ integrated operational amplifiers.
Further, the constant potentiometer comprises a first operational amplifier, a first resistor, a second resistor and a third resistor which are respectively connected with the negative input end of the first operational amplifier, the positive input end of the first operational amplifier is grounded to form a reverse addition circuit, the reverse addition circuit comprises three branches, the currents of the three branches are added at the negative input end of the first operational amplifier, and the sum of all the currents flowing in is zero.
Further, the three branches include:
A first branch: the input end of the first operational amplifier receives a control voltage EOUT, and acts on the reverse input end of the first operational amplifier through a first rheostat and the first resistor;
A second branch: the output end of the second operational amplifier is connected with the third resistor, a voltage follower is formed and is used as a feedback loop to be connected to a reference electrode, and a feedback signal of the reference electrode potential acts on the reverse input end of the first operational amplifier through the second operational amplifier and the third resistor;
Third branch: and a +5V reference source is externally connected in the circuit and is connected to the reverse input end of the first operational amplifier through a second rheostat and the second resistor so as to zero the system.
Further, the method further comprises the following steps: the first analog switch is connected with the output end of the first operational amplifier and one electrode of the electrolytic cell, the second analog switch is connected with the positive input end of the second operational amplifier and the other electrode of the electrolytic cell, and the third analog switch is connected with the IV conversion circuit and the other electrode of the electrolytic cell and is used for controlling whether the three electrode connecting ends of the potentiostat are connected with the electrolytic cell or not through the switch.
Further, the IV conversion circuit adopts a feedback type current measurement method, and comprises a third operational amplifier and a fourth operational amplifier, wherein the third operational amplifier and a feedback resistor form a current follower, the output voltage is in proportion to the polarized current, a polarized current signal to be measured is converted into a voltage signal, and the voltage parameter which is changed in phase with the control voltage EOUT is obtained through the fourth operational amplifier.
Further, the method further comprises the following steps: and the multipath analog switch is connected with the feedback resistor and is used for selecting and switching the feedback resistors with different resistance values.
Further, isolating and separately routing the power supply ground, digital ground and analog ground in the reverse-additive potentiostat and IV conversion measurement circuit includes isolating the analog power supply, analog components and analog ground from the digital power supply, digital components and digital ground.
The embodiment of the invention also provides an electrochemical measurement device, which comprises: the function generator, the reverse addition type constant potentiometer, the IV conversion measurement circuit, the receiving signal acquisition circuit and the microcontroller are provided by the embodiment, wherein the input end of the function generator is connected with the microcontroller, and the output end of the function generator is connected with the input ends of the high-precision reverse addition type constant potentiometer and the IV conversion measurement circuit and is used for generating required control voltage; the output end of the high-precision reverse addition type constant potentiometer and the output end of the IV conversion measurement circuit are connected with the receiving signal acquisition loop and are used for performing signal control and measurement according to the control voltage and converting polarized current output in the electrochemical reaction process into a voltage signal; the output end of the receiving signal acquisition loop is connected with the microcontroller and is used for receiving the measured signals.
Further, the function generator adopts a DA digital-to-analog converter, and the receiving signal acquisition loop adopts an AD analog-to-digital converter.
The reverse addition type potentiostat and the IV conversion measurement circuit for electrochemical measurement have the following beneficial effects:
(1) Under high-speed control voltage, the high-speed control voltage has higher stability and conversion precision;
(2) The current measurement resolution is high, and the repeatability is good;
(3) And a good anti-interference design is provided, so that the working stability of the circuit is ensured.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 is a schematic diagram of a reverse-additive potentiostat and an IV conversion measurement circuit according to an embodiment of the present invention;
FIG. 2 is a schematic circuit diagram of a potentiostat and its IV conversion according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of a sensitivity selection circuit according to an embodiment of the invention;
FIG. 4 is a schematic diagram of an anti-interference design according to an embodiment of the present invention;
Fig. 5 is a system block diagram of an electrochemical measurement device according to an embodiment of the present invention.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
As shown in fig. 1, the inverse-addition type potentiostat and IV-conversion measurement circuit according to an embodiment of the present invention includes: potentiostat 100, IV conversion circuit 200, electrolytic cell 300. In one embodiment of the present invention, the potentiostat 100 and the IV conversion circuit 200 each employ an integrated operational amplifier. The function generator adopts a DA digital-to-analog converter, and the receiving signal acquisition loop adopts an AD analog-to-digital converter.
In a general electrochemical reaction process, the maximum range of polarization current is mA level, and the current measurement resolution is less than 1nA. Common operational amplifiers have a current output capability of mA-stage. In order to prevent waveform distortion of the control voltage, important indicators to consider in the selection of the constant potentiometer 100 and the IV conversion circuit 200 are the input offset voltage, the input bias current, and the open loop gain. Therefore, the integrated chips AD8627 and AD8608 adopted in the potentiostat 100 and the IV conversion circuit 200 have input offset voltage of uV level, input bias current of pA level and open-loop gain exceeding 100Db, and meet the use requirement in the circuit.
Preferably, the potentiostat 100 is an integrated operational amplifier chip with the model AD 8627; the IV conversion circuit 200 is an integrated operational amplifier chip of model AD 8608.
Specifically, the positive input end of the potentiostat 100 is connected with the function generator, the reverse input and output ends of the potentiostat 100 are connected with the electrolytic cell 300, so that a closed loop of negative feedback amplification is formed by the potentiostat 100 and the electrolytic cell 300, the reference voltage is changed along with the adjustment of the control voltage, and is compared with the constant reference voltage of the working electrode to obtain a scanning voltage with the change range of +/-2V, and finally the polarized current output is realized.
Fig. 2 is a schematic circuit diagram of the potentiostat 100 and its IV conversion according to an embodiment of the present invention. Wherein WE, RE, CE represent working electrode, reference electrode and auxiliary electrode respectively, polarization current i is cathodic reduction current, and cathode current is defined as positive.
As shown in fig. 2, the potentiostat 100 includes a first operational amplifier A2, a first resistor R1, a second resistor R2 and a third resistor R3 respectively connected to negative input terminals of the first operational amplifier A2, and a positive input terminal of the first operational amplifier A2 is grounded to form a reverse addition circuit, which includes three branches, and currents of the three branches are added at the reverse input terminals of the first operational amplifier A2, and a sum of the currents flowing in the three branches is zero.
Specifically, the three branches include:
a first branch: the input end of the first operational amplifier A2 receives the control voltage EOUT, and acts on the reverse input end of the first operational amplifier A2 through the first rheostat RW1 and the first resistor R1;
A second branch: the output end of the second operational amplifier A2 is connected with a third resistor R3, and a voltage follower is formed and connected to the reference electrode as a feedback loop. Since the operational amplifier has a high input impedance, no large current flows on the reference electrode, thus avoiding interference with the electrode system being measured. The feedback signal of the reference electrode potential acts on the reverse input end of the first operational amplifier A2 through the second operational amplifier A1 and the third resistor R3.
Third branch: the external +5V reference source in the circuit is connected to the reverse input end of the first operational amplifier A2 through the second rheostat RW2 and the second resistor R2 to zero the system.
Specifically, the bias current and solution resistance of the operational amplifier in the loop have a certain influence on the control voltage, so that a +5V reference source externally connected in the circuit is connected to the reverse input end of the A2 through the rheostat RW2 and the resistor R2, and the system is zeroed. In this part of the circuit, the noninverting inputs of operational amplifiers A2 and A3 are the +2.5V reference source and are also the constant potential point of the working electrode. When the input signal EOUT changes between 1V and 4V, the voltage change range of the reference electrode is 4.5V-0.5V, and the potential change range of the equivalent working electrode relative to the reference electrode is-2V, so that the design requirement that the scanning voltage changes between +/-2V is met.
Referring to fig. 2, the negative input end of the IV conversion circuit 200 is connected to the electrolytic cell 300, the positive input end of the IV conversion circuit 200 is grounded, and the output end of the IV conversion circuit 200 is connected to a subsequent receiving signal acquisition circuit, so as to convert the polarized current output by the electrolytic cell 300 in the electrochemical reaction process into a voltage signal for data acquisition and processing by the subsequent receiving signal acquisition circuit.
Specifically, as shown in fig. 2, the IV conversion circuit 200 adopts a feedback current measurement method, which includes a third operational amplifier A3B and a fourth operational amplifier A3C, wherein the third operational amplifier A3B and the feedback resistor Rf form a current follower, the output voltage is proportional to the polarized current, the polarized current signal to be measured is converted into a voltage signal, and the voltage signal is passed through the fourth operational amplifier A3C to obtain a voltage parameter which is in-phase changed with the control voltage EOUT.
Specifically, the IV conversion circuit 200 converts the current flowing into the working electrode into a voltage signal for the AD acquisition loop to convert into a digital quantity. The invention adopts a feedback type current measurement method, the selected operational amplifier is an integrated chip AD8608 with 4 operational amplifiers inside, and 2 operational amplifiers in the circuit are respectively A3B and A3C. The current follower is formed by the operational amplifier A3B and the feedback resistor Rf, and the low bias current of the operational amplifier AD8608 has little influence on the polarized current i and can be ignored. Therefore, the output voltage of the third operational amplifier A3B is proportional to the polarized current, so that the polarized current signal to be measured is converted into a voltage signal, and the voltage parameter which is changed in phase with EOUT can be obtained through the fourth operational amplifier A3C. When the control voltage EOUT is changed between 1V and 4V, the output voltage range of the third operational amplifier A3B is measured to be 5V-0V, the output range of the third operational amplifier A3B is 0V-2.5V after passing through the inverse proportion operational circuit A3C, and the output voltage of the operational amplifier A3C is measured by the AD acquisition loop, so that the measurement and the recording of the polarized current can be realized.
In electrochemical analysis test, the polarization current to be tested is often different under different electrochemical system test conditions, so that a user is required to select proper sensitivity according to actual conditions, thereby ensuring the accuracy of current detection. Different feedback resistances Rf may be employed for different sensitivities. In one embodiment of the present invention, further comprising: and the multipath analog switches are connected with the feedback resistors and are used for selecting and switching the feedback resistors with different resistance values.
Preferably, the multi-path analog switch is MAX4617.
Specifically, the multi-path analog switch MAX4617 is adopted to realize the switching of Rf, and the filter capacitor Cf is connected in parallel to the two ends of Rf to form a low-pass filter, the schematic diagram is shown in figure 3, and the circuit of the part is connected to figure 2 through IWE and OWE endpoints to replace the Rf and Cf loops in figure 2.
In addition, as shown in fig. 2, the present invention further includes: first to third analog switches, the first analog switch is connected to the output terminal of the first operational amplifier and one electrode of the electrolytic cell 300, the second analog switch is connected to the positive input terminal of the second operational amplifier and the other electrode of the electrolytic cell 300, and the third analog switch is connected to the IV conversion circuit 200 and the other electrode of the electrolytic cell 300 for controlling the conduction or non-conduction of the three electrode connection terminals of the potentiostat 100 and the electrolytic cell 300 through the switches.
Specifically, to control the test process, it is also necessary to control the conduction between the three electrode connection terminals of the potentiostat 100 and the electrolytic cell 300 through a switch. To achieve this function, the first to third analog switches in the present circuit use DG419 with low on-resistance and fast response. As shown in fig. 2, the first to third analog switches are D1, D2, and D3, respectively. Because the operational amplifier has very small output impedance, an AD acquisition circuit can be externally connected to the output end of the operational amplifier A1, so that the real-time measurement and recording of the scanning voltage are realized.
The whole loop of the invention is composed of an analog device and a part of analog device controlled by digital signals, and the analog device has poor anti-interference performance, so that the isolation and the separate wiring of the power supply ground, the digital ground and the analog ground and the isolation of the power supply are carried out when the PCB design is carried out. As shown in fig. 5, the isolation and separate wiring of the power supply ground, digital ground and analog ground in the inverse-addition type potentiostat 100 and the IV conversion measurement circuit includes the isolation of the analog power supply, analog element and analog ground from the digital power supply, digital element and digital ground by magnetic beads, realizing the anti-interference design.
As shown in fig. 5, an electrochemical measurement device according to an embodiment of the present invention includes: the function generator 2, the reverse addition type potentiostat and the IV conversion measurement circuit 1 provided by the embodiment, the receiving signal acquisition circuit 3 and the microcontroller 4.
Specifically, the input end of the function generator 2 is connected with the microcontroller 4, and the output end of the function generator 2 is connected with the input end of the high-precision inverse addition type potentiostat and the IV conversion measurement circuit 1, so as to generate the required control voltage. The output end of the high-precision reverse addition type constant potentiometer and IV conversion measurement circuit 1 is connected with a receiving signal acquisition loop 3 and is used for performing signal control and measurement according to control voltage and converting polarized current output in the electrochemical reaction process into a voltage signal. The output end of the receiving signal acquisition loop 3 is connected with the microcontroller and is used for receiving the measured signals. The microcontroller 4 mainly adopts an embedded microprocessor as a main controller to realize the functions of automatic control, data acquisition, data processing, display, transmission and the like.
In one embodiment of the invention, the function generator 2 employs a DA digital-to-analog converter, and the receive signal acquisition loop 3 employs an AD analog-to-digital converter.
The reverse addition type potentiostat and the IV conversion measurement circuit for electrochemical measurement have the following beneficial effects:
(1) Under high-speed control voltage, the high-speed control voltage has higher stability and conversion precision;
(2) The current measurement resolution is high, and the repeatability is good;
(3) And a good anti-interference design is provided, so that the working stability of the circuit is ensured.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives, and variations may be made in the above embodiments by those skilled in the art without departing from the spirit and principles of the invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A reverse-additive potentiostat and IV-conversion measurement circuit, comprising: the device comprises a potentiostat, an IV conversion circuit and an electrolytic cell, wherein the positive input end of the potentiostat is connected with a function generator, and the reverse input and output ends of the potentiostat are connected with the electrolytic cell so as to form a closed loop of negative feedback amplification by the potentiostat and the electrolytic cell and output polarized current; the negative input end of the IV conversion circuit is connected with the electrolytic cell, the positive input end of the IV conversion circuit is grounded, and the output end of the IV conversion circuit is connected with a subsequent receiving signal acquisition loop and is used for converting polarized current output by the electrolytic cell in the electrochemical reaction process into a voltage signal for data acquisition and processing of the subsequent receiving signal acquisition loop; the constant potential device comprises a first operational amplifier, a first resistor, a second resistor and a third resistor, wherein the first resistor, the second resistor and the third resistor are respectively connected with the negative input end of the first operational amplifier, the positive input end of the first operational amplifier is grounded to form a reverse addition circuit, and the reverse addition circuit comprises three branches;
The three branches include: a first branch: the input end of the first operational amplifier receives a control voltage EOUT, and acts on the reverse input end of the first operational amplifier through a first rheostat and the first resistor; a second branch: the output end of the second operational amplifier is connected with the third resistor, a voltage follower is formed and is used as a feedback loop to be connected to a reference electrode, and a feedback signal of the reference electrode potential acts on the reverse input end of the first operational amplifier through the second operational amplifier and the third resistor; third branch: a +5V reference source is externally connected in the circuit and connected to the reverse input end of the first operational amplifier through a second rheostat and the second resistor so as to zero the system;
the currents of the three branches are added at the reverse input end of the first operational amplifier, and the sum of all the currents flowing in is zero;
Further comprises: the first analog switch is connected with the output end of the first operational amplifier and one electrode of the electrolytic cell, the second analog switch is connected with the positive input end of the second operational amplifier and the other electrode of the electrolytic cell, and the third analog switch is connected with the IV conversion circuit and the other electrode of the electrolytic cell and is used for controlling the connection end of the three electrodes of the potentiostat and the electrolytic cell to be conducted or not through the switch;
The IV conversion circuit adopts a feedback type current measurement method and comprises a third operational amplifier and a fourth operational amplifier, wherein the third operational amplifier and a feedback resistor form a current follower, the output voltage is in proportion to the polarized current, a polarized current signal to be measured is converted into a voltage signal, and the voltage parameter which is in-phase changed with the control voltage EOUT is obtained through the fourth operational amplifier.
2. The inverse-additive potentiostat and IV conversion measurement circuit of claim 1, wherein the potentiostat and IV conversion circuit each employ an integrated operational amplifier.
3. The reverse-additive potentiostat and IV conversion measurement circuit of claim 1, further comprising: and the multipath analog switch is connected with the feedback resistor and is used for selecting and switching the feedback resistors with different resistance values.
4. The reverse-additive potentiostat and IV conversion measurement circuit of claim 1, wherein isolating and separately wiring the power ground, digital ground, and analog ground in the reverse-additive potentiostat and IV conversion measurement circuit comprises isolating the analog power source, analog components, and analog ground from the digital power source, digital components, and digital beads.
5. An electrochemical measurement device, comprising: the function generator, the reverse addition type potentiostat and IV conversion measurement circuit according to any one of claims 1-4, a received signal acquisition loop and a microcontroller, wherein the input end of the function generator is connected with the microcontroller, and the output end of the function generator is connected with the input end of the high-precision reverse addition type potentiostat and IV conversion measurement circuit and is used for generating required control voltage; the output end of the high-precision reverse addition type constant potentiometer and the output end of the IV conversion measurement circuit are connected with the receiving signal acquisition loop and are used for performing signal control and measurement according to the control voltage and converting polarized current output in the electrochemical reaction process into a voltage signal; the output end of the receiving signal acquisition loop is connected with the microcontroller and is used for receiving the measured signals.
6. The electrochemical measurement device of claim 5, wherein the function generator employs a DA digital-to-analog converter and the receive signal acquisition loop employs an AD analog-to-digital converter.
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| CN111693582A (en) * | 2020-05-26 | 2020-09-22 | 杭州电子科技大学 | Portable front end device of electrochemistry detection high accuracy |
| CN115484868A (en) * | 2020-06-30 | 2022-12-16 | 浙江大学 | Constant potential circuit, blood sugar measurement circuit and equipment |
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