CN109444245B - Calibration system and calibration method of cyclic voltammetry analyzer - Google Patents
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Abstract
The invention provides a calibration system and a calibration method of a cyclic voltammetry analyzer, and belongs to the field of electroplating. The method aims to solve the technical problems that the accuracy of the quantity value tracing cannot be effectively guaranteed and the metering characteristics cannot be evaluated because the metering performance of a cyclic voltammetry analyzer has no special calibration regulation, calibration standard and other standards in the prior art. The invention provides a calibration system and a calibration method of a cyclic voltammetry analyzer, which can calibrate parameters of the cyclic voltammetry stripping analyzer and comprehensively evaluate the metering characteristics of the cyclic voltammetry stripping analyzer.
Description
Technical Field
The invention relates to the field of electroplating, in particular to a calibration system and a calibration method of a cyclic voltammetry analyzer.
Background
At present, a cyclic voltammetry, namely a Cyclic Voltammetry (CVS) analyzer is basically adopted by a plating solution additive analyzer, and can be used for analyzing organic matters and pollutants in electroplating. The additives in the bath ultimately affect the ductility, tensile strength, and even final solderability of the wiring board metal coating. The method is used for analysis and test of electroplating additives (light agents and leveling agents), is mainly used for electroplating bath analysis, and is widely applied to circuit boards, semiconductors, precise electroplating, solar electroplating and the like with higher requirements on electroplating control. The normalized inspection of organic additives is an important means for ensuring the quality of products.
The electrolytic cell is a place where electroplating takes place, and can convert electric energy into chemical energy, and consists of an external power supply, an electrolyte solution and electrodes participating in working:
the cathode of the device is as follows: obtaining electrons, carrying out reduction reaction, and connecting the electrode with a negative electrode of a power supply;
anode: losing electrons, carrying out oxidation reaction and connecting with the anode of a power supply;
in the cell, current flows from the anode to the cathode.
If the electrode reaction is O + e- → R, the solution only contains the reactive particles O before the reaction, O, R is soluble in the solution, the scanning starting potential is controlled to be in forward direction electric scanning from the starting potential (phi i) which is much more positive than the standard equilibrium potential (phi flat) of the system, and the current response curve is shown in the attached figure 1.
When the electrode potential gradually moves negative to near (phi-flat), O starts to reduce on the electrode and i-faradaic passes through. As the potential becomes more negative, the concentration of reactant O at the electrode surface gradually decreases, and thus the flow and current to the electrode surface increases. When the surface concentration of O drops to near zero, the current also increases to a maximum IpcThen, the current gradually decreases. When the potential reaches (phi r), the scanning is reversed.
As the electrode potential becomes more positive, the concentration of oxidizable R particles near the electrode is greater and the electrochemical equilibrium at the surface should progress more and more in favor of R generation as the potential approaches and passes (phi flat). Whereupon R begins to oxidize and the current increases to a peak oxidation current IpaWhich in turn causes a current decay due to the significant consumption of R. The entire curve is called a "cyclic voltammogram".
The cyclic voltammetry analyzer is important instrument equipment for analyzing the electroplating solution additive in the manufacturing industry, can provide powerful technical support for environment-friendly green manufacturing, and is wide in market application, but the measurement performance of the cyclic voltammetry analyzer does not have standards such as special verification rules and calibration standards in the industry at present, the accuracy of tracing the measurement value cannot be effectively guaranteed, and the measurement characteristic cannot be evaluated, so that the measurement calibration of the cyclic voltammetry analyzer needs to be researched.
Disclosure of Invention
The invention aims to provide a calibration system and a calibration method of a cyclic voltammetry analyzer, so as to solve the problem that the magnitude of the cyclic voltammetry analyzer cannot be traced.
In order to solve the problems, the invention provides a calibration system of a cyclic voltammetry analyzer.
A calibration system of a cyclic voltammetry analyzer comprises a computer, a single chip microcomputer, a voltage measurement module, a first impedance module, a second impedance module, a multi-way conversion switch module, a wiring terminal 1, a wiring terminal 2 and a wiring terminal 3. Wherein:
the terminal 1 is used for connecting a working electrode of the calibrated cyclic voltammetry analyzer and is connected with a first port of the first impedance module;
the terminal 2 is used for connecting a reference electrode of the calibrated cyclic voltammetry analyzer and is connected with the second port of the first impedance module and the first port of the second impedance module;
the terminal 3 is used for connecting a reference electrode of the calibrated cyclic voltammetry analyzer and is connected with a second port of the second impedance module;
the multi-way switch module is connected with the voltage measuring module, the single chip microcomputer, the wiring terminal 1, the wiring terminal 2 and the wiring terminal 3, and the multi-way switch module can enable the voltage measuring module to detect the potential difference between the two ends of the first impedance module or the second impedance module under the control of the single chip microcomputer;
the computer is connected with the singlechip, and the singlechip controls the multi-way switch module under the control of the computer;
the computer receives the measurement data of the voltage measurement module obtained by sampling through the single chip microcomputer, processes the measurement data and generates a final calibration report.
The invention also provides a calibration method of the cyclic voltammetry analyzer on the calibration system, which can obtain the voltage relative indicating value error and the current relative indicating value error of the cyclic voltammetry analyzer,
the method comprises the following steps of obtaining a voltage relative indicating value error:
disconnecting a working electrode, a reference electrode and an auxiliary electrode of the cyclic voltammetry analyzer to be calibrated;
the terminal 1 of the calibration system is connected with a working electrode of the cyclic analyzer to be calibrated; the terminal 2 of the calibration system is connected with a reference electrode of the cyclic analyzer to be calibrated; the terminal 3 of the calibration system is connected with an auxiliary electrode of the cyclic analyzer to be calibrated;
the computer sends a control instruction to the single chip microcomputer, and the single chip microcomputer drives the multi-path conversion module to enable the voltage measurement module to measure the potential difference at the two ends of the first impedance module;
setting the voltage output of the cyclic voltammetry analyzer to be calibrated, uniformly selecting not less than 5 calibration points in the voltage range measured by the cyclic voltammetry analyzer, and recording the voltage value U of the cyclic voltammetry analyzer to be calibratedXAnd voltage reading value U of voltage measuring moduleSThe computer records the test data of the voltage test module through the singlechip;
calculating voltage relative indication error:
wherein: deltaUThe voltage relative indicating value error is obtained; u shapeXIndicating the voltage value of the calibrated cyclic voltammetry analyzer; u shapeSThe voltage indication value of the voltage measurement module is shown.
On the other hand, the step of obtaining the current relative indicating value error comprises the following steps:
disconnecting a working electrode, a reference electrode and an auxiliary electrode of the cyclic voltammetry analyzer to be calibrated;
connecting a terminal 1 of the calibration system to a working electrode of the cyclic analyzer to be calibrated; connecting terminal 2 of the calibration system to the reference electrode of the cyclic analyzer to be calibrated; connecting the terminal 3 of the calibration system to the auxiliary electrode of the calibration cycle analyzer;
the computer sends a control instruction to the single chip microcomputer, and the single chip microcomputer drives the multi-path conversion module to enable the voltage measurement module to measure the potential difference at the two ends of the second impedance module;
setting calibrated voltage output U of cyclic voltammetry analyzerb(general output 1V), change the external impedance R of the first impedance module1The external impedance R of the second standard impedance module2Thereby changing the current passing through the working electrode and the auxiliary electrode and recording the current value I of the calibrated cyclic voltammetry analyzerXAnd voltage reading value U of voltage measuring moduleSAnd the computer records the test data of the voltage test module through the singlechip.
Calculating the relative indicating value error of the current:
wherein: deltaIThe current relative indicating value error is obtained; i isXCurrent indicating values of the calibrated cyclic voltammetry analyzer; r2Is the resistance value of the second impedance module; u shapeSThe voltage indication value of the voltage measurement module is shown.
Further, according to the results obtained by the calibration method, the linearity error and repeatability of the cyclic voltammetry analyzer are further evaluated.
In the following, a method for calibrating the linearity error of a cyclic voltammetric analyzer is described:
step 21), adjusting all parameters of the cyclic voltammetry analyzer to a normal working state, and calibrating according to a 10mL/L series standard solution (if a standard solution with an intermediate concentration point is used according to other concentrations) used in the specification of the cyclic voltammetry analyzer;
step 22), recording measurement results c) by using a cyclic voltammeter to respectively measure series of standard solutions with other concentrationsi；
Step 23), calculating the linearity error as follows:
wherein: deltaiLinearity error for the ith concentration measurement; c. CiInstrumental measurements for the ith concentration standard solution; c. CsiIs the standard value of the ith concentration standard solution; and taking the linear error value with the maximum absolute value as the linear error of the cyclic voltammetry analyzer.
The following describes the calibration method for the repeatability of the cyclic voltammetry analyzer:
step 31), adjusting all parameters of the cyclic voltammetry analyzer to a normal working state, executing step 21) and step 22 every time, and measuring the concentration of 10mL/L series standard solution (if the standard solution with the minimum concentration to be measured is prepared according to other concentrations) for 3 times;
step 32), calculating the measurement repeatability according to the following formula:
wherein: delta is the measurement repeatability; c. Cmax、cminThe maximum value and the minimum value of the 3 measurement results are obtained;
the average of 3 measurements.
According to the calibration system and the calibration method of the cyclic voltammetry analyzer, provided by the invention, the calibration of the electrical parameters of the cyclic voltammetry analyzer, such as voltage relative indicating value errors, current relative indicating value errors and linear errors, can be realized, and the cyclic voltammetry analyzer is evaluated through repeated verification. Finally, the source tracing of the cyclic voltammetry analyzer is realized, and compared with the prior art, the method can calibrate and comprehensively evaluate the electrical parameters of the cyclic voltammetry analyzer.
Drawings
FIG. 1 is a plot of the sweep current response of cyclic voltammetry;
FIG. 2 is a calibration system for a cyclic voltammetric analyzer of the present invention;
FIG. 3 is a voltage calibration connection diagram of the calibration system of the present invention;
fig. 4 is a current calibration connection diagram of the calibration system of the present invention.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The cyclic voltammetry analyzer is important instrument and equipment for analyzing the electroplating solution additive in the manufacturing industry, can provide powerful technical support for environment-friendly and green manufacturing, and is wide in market application. However, in the prior art, no standards such as special verification rules and calibration standards exist for the metering performance, the accurate source tracing of the quantity value cannot be effectively guaranteed, and the metering characteristics cannot be evaluated.
The application provides a calibration system of a cyclic voltammetry analyzer.
FIG. 2 is a connection diagram of a calibration system of a cyclic voltammetric analyzer according to the present invention. Wherein:
a calibration system of cyclic voltammetry analyzer, characterized in that: the device comprises a computer, a single chip microcomputer, a voltage measuring module, a first impedance module, a second impedance module, a multi-way conversion switch module, a wiring terminal 1, a wiring terminal 2 and a wiring terminal 3. Wherein:
the terminal 1 is used for connecting a working electrode of the calibrated cyclic voltammetry analyzer and is connected with a first port of the first impedance module;
the terminal 2 is used for connecting a reference electrode of the calibrated cyclic voltammetry analyzer and is connected with the second port of the first impedance module and the first port of the second impedance module;
the terminal 3 is used for connecting a reference electrode of the calibrated cyclic voltammetry analyzer and is connected with a second port of the second impedance module;
the multi-way switch module is connected with the voltage measuring module, the single chip microcomputer, the wiring terminal 1, the wiring terminal 2 and the wiring terminal 3, and the multi-way switch module can enable the voltage measuring module to detect the potential difference on the first impedance module or the second impedance module under the control of the single chip microcomputer;
the computer is connected with the singlechip, and the singlechip controls the multi-way switch module under the control of the computer;
the computer receives the measurement data of the voltage measurement module obtained by sampling through the single chip microcomputer, processes the measurement data and generates a final calibration report.
The first impedance module and the second impedance module can be modules formed by connecting a multi-way gating switch and a standard resistor array in series: at the moment, the multi-path gating switch is connected with the single chip microcomputer, and under the control of the single chip microcomputer, the multi-path gating switch gates only one specific standard resistor in the resistor array, so that the external impedance of the impedance module is the same as the resistance value of the specific standard resistor.
The first impedance block and the second impedance block may also be a single variable resistor.
Preferably, the resistance value of the variable resistor is varied in a range of 10K Ω to 20K Ω; the standard resistor array comprises standard resistors with the resistance values of 10K omega, 12K omega, 14K omega, 16K omega, 18K omega and 20K omega; the standard resistor array comprises N resistors, the minimum value of the N resistors is 10K omega, the maximum value of the N resistors is 20K omega, and the impedance of the N resistors forms an arithmetic progression standard resistor.
Wherein, the external impedances of the first impedance module and the second impedance module are respectively marked as R1、R2。
In order to realize the comprehensive evaluation of the characteristics of the voltammetry analyzer, based on the calibration system of the voltammetry analyzer, the calibration is respectively carried out from the voltage relative indicating value error, the current relative indicating value error, the linear error and the repeatability of the cyclic voltammetry analyzer, and the electrical parameters of the voltammetry analyzer are comprehensively analyzed and calibrated.
Firstly, the voltage relative indicating value error calibration step of the calibration system is introduced:
step 1), disconnecting a working electrode, a reference electrode and an auxiliary electrode of a cyclic voltammetry analyzer to be calibrated;
step 2), connecting a terminal 1 of the calibration system with a working electrode of the calibrated cyclic analyzer; the terminal 2 of the calibration system is connected with a reference electrode of the cyclic analyzer to be calibrated; the terminal 3 of the calibration system is connected with an auxiliary electrode of the cyclic analyzer to be calibrated; the connection mode is shown in figure 3;
step 3), sending a control instruction to the single chip microcomputer by the computer, and driving the multi-path conversion module by the single chip microcomputer to enable the voltage measurement module to measure the potential difference at the two ends of the first impedance module;
step 4), setting the calibratedOutputting voltage of the cyclic voltammetry analyzer, uniformly selecting not less than 5 calibration points in the voltage range measured by the cyclic voltammetry analyzer, and recording the voltage value U of the cyclic voltammetry analyzer to be calibratedXAnd voltage reading value U of voltage measuring moduleSThe computer records the test data of the voltage test module through the singlechip;
and step 5), calculating the voltage relative indicating value error according to the formula (1):
wherein: deltaUThe voltage relative indicating value error is obtained; u shapeXIndicating the voltage value of the calibrated cyclic voltammetry analyzer; u shapeSThe voltage indication value of the voltage measurement module is shown.
Then, a method for calibrating the current relative indication error of the system is introduced:
step 11), disconnecting a working electrode, a reference electrode and an auxiliary electrode of the cyclic voltammetry analyzer to be calibrated;
step 12), connecting the terminal 1 of the calibration system to a working electrode of the calibrated cyclic analyzer; connecting terminal 2 of the calibration system to the reference electrode of the cyclic analyzer to be calibrated; connecting the terminal 3 of the calibration system to the auxiliary electrode of the calibration cycle analyzer; the connection mode is shown in figure 4;
step 13), the computer sends a control instruction to the single chip microcomputer, and the single chip microcomputer drives the multi-path conversion module to enable the voltage measurement module to measure the potential difference at the two ends of the second impedance module;
step 14), setting the voltage output U of the calibrated cyclic voltammetry analyzerb(general output 1V), change the external impedance R of the first impedance module1The external impedance R of the second standard impedance module2Thereby changing the current passing through the working electrode and the auxiliary electrode and recording the current value I of the calibrated cyclic voltammetry analyzerXAnd voltage reading value U of voltage measuring moduleSAnd the computer records the test data of the voltage test module through the singlechip.
Step 15), calculating the relative indicating value error of the current according to the formula (2):
wherein: deltaIThe current relative indicating value error is obtained; i isXCurrent indicating values of the calibrated cyclic voltammetry analyzer; r2Is the resistance value of the second impedance module; u shapeSThe voltage indication value of the voltage measurement module is shown.
Preferably, the order of the voltage relative indication error calibration step and the current relative indication error calibration step can be reversed.
After the voltage relative indicating value error and the current relative indicating value error of the cyclic voltammetry analyzer are obtained, the concentration of the specific solution can be obtained according to a known standard cyclic voltammogram of the specific solution; and further evaluating the linearity error and the repeatability of the cyclic voltammetry analyzer.
In the following, a method for calibrating the linearity error of a cyclic voltammetric analyzer is described:
step 21), adjusting all parameters of the cyclic voltammetry analyzer to a normal working state, and calibrating according to a 10mL/L series standard solution (if a standard solution with an intermediate concentration point is used according to other concentrations) used in the specification of the cyclic voltammetry analyzer;
step 22), recording measurement results c) by using a cyclic voltammeter to respectively measure series of standard solutions with other concentrationsi；
Step 23), calculating a linear error according to the following formula (3):
wherein: deltaiLinearity error for the ith concentration measurement; c. CiInstrumental measurements for the ith concentration standard solution; c. CsiIs the standard value of the ith concentration standard solution; and taking the linear error value with the maximum absolute value as the linear error of the cyclic voltammetry analyzer.
The following describes the calibration method for the repeatability of the cyclic voltammetry analyzer:
step 31), adjusting all parameters of the cyclic voltammetry analyzer to a normal working state, executing step 21) and step 22 every time, and measuring the concentration of 10mL/L series standard solution (if the standard solution with the minimum concentration to be measured is prepared according to other concentrations) for 3 times;
step 32), calculating the measurement repeatability according to the formula (4):
wherein: delta is the measurement repeatability; c. Cmax、cminThe maximum value and the minimum value of the 3 measurement results are obtained;
the average of 3 measurements.
By using the repeatability test, the influence of uncontrollable factors on a calibration result in the operation process can be reduced.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.
Claims (7)
1. A calibration system of cyclic voltammetry analyzer, characterized in that: the device comprises a computer, a singlechip, a voltage measuring module, a first impedance module, a second impedance module, a multi-way conversion switch module, a wiring terminal 1, a wiring terminal 2 and a wiring terminal 3;
the terminal 1 is used for connecting a working electrode of the calibrated cyclic voltammetry analyzer and is connected with a first port of the first impedance module;
the terminal 2 is used for connecting a reference electrode of the calibrated cyclic voltammetry analyzer and is connected with the second port of the first impedance module and the first port of the second impedance module;
the terminal 3 is used for connecting an auxiliary electrode of the calibrated cyclic voltammetry analyzer and is connected with a second port of the second impedance module;
the multi-way conversion switch module is connected with the voltage measurement module, the single chip microcomputer, the wiring terminal 1, the wiring terminal 2 and the wiring terminal 3, and under the control of the single chip microcomputer, the multi-way conversion switch module can enable the voltage measurement module to detect the potential difference between two ends of the first impedance module or the second impedance module;
the computer is connected with the singlechip, and the singlechip controls the multi-path change-over switch module under the control of the computer;
the computer receives the measurement data of the voltage measurement module obtained by sampling through the singlechip, and the computer processes the measurement data and generates a final calibration report;
the first impedance module and the second impedance module are modules formed by connecting a multi-way gating switch and a standard resistor array in series or single variable resistors:
the multi-path gating switch is connected with the single chip microcomputer;
the multi-path gating switch gates only one specific standard resistor in the resistor array under the control of the single chip microcomputer, so that the external impedance of the impedance module is the same as the resistance value of the specific standard resistor.
2. The calibration system according to claim 1, wherein the variable resistor has a resistance value ranging from 10K Ω to 20K Ω.
3. The calibration system of claim 2, wherein: the standard resistor array comprises standard resistors with the resistance values of 10K omega, 12K omega, 14K omega, 16K omega, 18K omega and 20K omega.
4. A method of calibrating a calibration system according to any one of claims 1 to 3, characterized by: the method comprises the steps of acquiring a voltage relative indicating value error:
step 1), disconnecting a working electrode, a reference electrode and an auxiliary electrode of a cyclic voltammetry analyzer to be calibrated;
step 2), connecting the terminal 1 of the calibration system to a working electrode of the calibrated cyclic analyzer; connecting terminal 2 of the calibration system to the reference electrode of the cyclic analyzer to be calibrated; connecting the terminal 3 of the calibration system to the auxiliary electrode of the cyclic analyzer to be calibrated;
step 3), the computer sends a control instruction to the single chip microcomputer, and the single chip microcomputer drives the multi-path conversion module to enable the voltage measurement module to measure the potential difference at the two ends of the first impedance module;
step 4), setting the voltage output of the cyclic voltammetry analyzer to be calibrated, uniformly selecting not less than 5 calibration points in the voltage range measured by the cyclic voltammetry analyzer, and recording the voltage value U of the cyclic voltammetry analyzer to be calibratedXAnd voltage reading value U of voltage measuring moduleSThe computer records the test data of the voltage test module through the singlechip;
and step 5), calculating the voltage relative indicating value error according to the following formula:
wherein: deltaUThe voltage relative indicating value error is obtained; u shapeXIndicating the voltage value of the calibrated cyclic voltammetry analyzer; u shapeSIndicating the voltage of the voltage measuring module;
and acquiring the concentration of the specific solution according to a standard cyclic voltammogram of the specific solution, and evaluating the linearity error and repeatability of the cyclic voltammetry analyzer.
5. A method of calibrating a calibration system according to claim 4, characterized by: the step of obtaining the voltage relative indicating value error further comprises the step of obtaining the current relative indicating value error:
step 11), disconnecting a working electrode, a reference electrode and an auxiliary electrode of the cyclic voltammetry analyzer to be calibrated;
step 12), connecting the terminal 1 of the calibration system to a working electrode of the calibrated cyclic analyzer; connecting terminal 2 of the calibration system to the reference electrode of the cyclic analyzer to be calibrated; connecting the terminal 3 of the calibration system to the auxiliary electrode of the calibration cycle analyzer;
step 13), the computer sends a control instruction to the single chip microcomputer, and the single chip microcomputer drives the multi-path conversion module to enable the voltage measurement module to measure the potential difference at the two ends of the second impedance module;
step 14), setting the voltage output U of the calibrated cyclic voltammetry analyzerbChanging the external impedance R of the first impedance module1The external impedance R of the second standard impedance module2Thereby changing the current passing through the working electrode and the auxiliary electrode and recording the current value I of the calibrated cyclic voltammetry analyzerXAnd voltage reading value U of voltage measuring moduleSThe computer records the test data of the voltage test module through the singlechip;
step 15), calculating the relative indicating value error of the current by the following formula:
wherein: deltaIThe current relative indicating value error is obtained; i isXCurrent indicating values of the calibrated cyclic voltammetry analyzer; r2Is the resistance value of the second impedance module; u shapeSThe voltage indication value of the voltage measurement module is shown.
6. A method of calibrating a calibration system according to claim 5, characterized by: further comprising a linear error analysis step:
step 21), adjusting all parameters of the cyclic voltammetry analyzer to a normal working state, and calibrating the used 10mL/L series standard solution according to the specification of the cyclic voltammetry analyzer;
step 22), recording measurement results c) by using a cyclic voltammeter to respectively measure series of standard solutions with other concentrationsi；
Step 23), calculating a linearity error by the following formula:
wherein: deltaiLinearity error for the ith concentration measurement; c. CiInstrumental measurements for the ith concentration standard solution; c. CsiIs the standard value of the ith concentration standard solution; and taking the linear error value with the maximum absolute value as the linear error of the cyclic voltammetry analyzer.
7. A method of calibrating a calibration system according to claim 4 or 5, further characterized by the steps of: the method also comprises a method for calibrating the repeatability of the cyclic voltammetry analyzer:
step 31), adjusting all parameters of the cyclic voltammetry analyzer to a normal working state, and executing the step 21) and the step 22) each time, and measuring the concentration of 10mL/L series standard solution for 3 times;
step 32), calculating the measurement repeatability according to the following formula:
wherein: delta is the measurement repeatability; c. Cmax、cminThe maximum value and the minimum value of the 3 measurement results are obtained;
the average of 3 measurements.
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Address after: No. 8 Qishan Road, Shiqi Town, Panyu District, Guangzhou City, Guangdong Province, 510000, 150 Patentee after: Radio and TV Measurement and Testing Group Co.,Ltd. Patentee after: GRGT METERING DETECTION (NANNING) Co.,Ltd. Address before: 510630 Xiping Road, Whampoa Road, Tianhe District, Guangzhou, Guangdong 163 Patentee before: GUANGZHOU GRG METROLOGY & TEST Co.,Ltd. Patentee before: GRGT METERING DETECTION (NANNING) Co.,Ltd. |