CN104020214B - A kind of assay method of electrode reaction parameter - Google Patents
A kind of assay method of electrode reaction parameter Download PDFInfo
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Abstract
The present invention is to provide a kind of assay method of electrode reaction parameter. By three electrode access electrochemical workstations of three-electrode system reaction unit, use cyclic voltammetry to measure primary data, primary data is processed, obtain electrochemical reaction parameters and data relationship figure; Primary data is processed and comprised: read in first in batches file, then the data that adopt four layer data structures storages to read in, and from file name, read the information of temperature and sweep speed, after all reading in and storing, carry out Data correction and pretreatment, and then draw according to the result after proofreading and correct, judge reaction type, and obtain diffusion coefficient, reaction activity, speed constant data in conjunction with computing formula, finally demonstrate result of calculation and picture. The present invention can record electrode reaction dynamics and thermodynamic parameter easily, greatly shortens determination period, reduces overall workload, and overall cost is cheap, and final calculation result can meet most of needs with the figure of drawing.
Description
Technical field
The present invention relates to a kind of method of measuring electrode reaction parameter, particularly used cyclic voltammetry electrode reaction parameterMethod.
Background technology
Many electrode reactions are subject to material DIFFUSION CONTROLLED, and diffusion is that dissufion current is anti-because the gradient of an electrochemical potential is causedAnswer the diffusion part of electroactive material at electrode surface flow. In microcosmic viewpoint-discontinuous source model, think diffusion coefficient D0OneThe individual constant relevant with step-length and step frequency, then in conjunction with Fick's law, we just can know after diffusion coefficient having obtainedThe time dependent rule of reactant concentration, for instructing us to select best reaction condition. Reaction rate constant has reacted changeLearn the speed that carries out of reaction, calculate reaction rate constant and can know the minimizing of electrode surface reactant concentration in the unit intervalOr the recruitment of product concentration. Find applicable reaction condition to control electrochemical reaction, accelerate reaction rate, with increasingLearn the output of product. Calculate reaction activity can instruct endothermic heat of reaction or heat release number, knowing reaction activationCan offer theoretical foundation for we select optimization reaction, produce and scientific and technical requirement to meet.
Diffusion coefficient is thermodynamic data, and reaction rate constant and reaction activity are basic dynamics datas. These basesChemical reaction data can be for analyzing electrode reaction mechanism and rule, and therefore obtaining these basic electrode response datas and be one mustThe basic research work of palpus.
Cyclic voltammetry is research method very important in electrochemical field. The method, by control electrode electromotive force, adopts differentSpeed with once or repeatedly scanning repeatedly of triangular waveform, potential change makes, on electrode, different reduction and oxidation alternately to occurReaction, and record current potential curve. Cyclic voltammetry obtains cyclic voltammetry curve, can judge that according to curve shape electrode is anti-Degree of reversibility, intermediate, phase boundary absorption or the possibility of New phase formation and the character of coupled chemical reactions etc. of answering. Pass throughTo the analysis of cyclic voltammetry curve, can calculate diffusion coefficient D0, reaction activity Ea, rate constants ksDeng. But useData that cyclic voltammetry obtains are scattered and data volume is larger, post-processed difficulty. At present, general later data is processed and is allThe method that adopts Excel to calculate or combine with function software by some data processing softwares. These methods have some and lackPoint:
(1) rely on data processing software as Origin or MATLAB expensive.
(2) data processing software version is more, may cause the problem incompatible with function software and cannot use.
(3) function software and data processing software some do not there is cross-platform function, can only be used for part operation system, partComputer cannot use.
(4) data also need manually input or adjust (as oxidation peak reduction peak current current potential), have increased workload with artificialError, result of calculation accuracy depends on operator's level professional technology.
Open source literature related to the present invention comprises:
[1] Ma Yalin, Shen Ningyi, Yin Aijun, Huang is set the mind on study. cyclic voltammetry data acquisition and processing system [J]. University Of Xiangtan's natureScience journal, 2000,6;
[2] Mo Lingzhi, Wang Rulong, Zhang Jin. design and the realization of the electrochemistry experiment data handling system based on VB and Matlab[J]. computer and applied chemistry, 2011,28 (2): 253-256.
Summary of the invention
The object of the present invention is to provide a kind of electrode reaction parameter that can record easily electrochemical reaction parameters and reduce workloadAssay method.
The object of the present invention is achieved like this:
By three electrode access electrochemical workstations of three-electrode system reaction unit, use cyclic voltammetry to measure primary data,Primary data is processed, obtained electrochemical reaction parameters and data relationship figure; Described primary data is processed specificallyComprise: read in file first in batches, the data that then adopt four layer data structures storages to read in, and from file name, read temperatureDegree and the information of sweep speed, after all reading in and storing, carry out Data correction and pretreatment, and then according to after correctionResult is drawn, and judges reaction type, and obtains diffusion coefficient, reaction activity, speed constant data in conjunction with computing formula,Finally demonstrate result of calculation and picture.
The present invention can also comprise:
1, described use cyclic voltammetry is measured primary data and is specifically comprised: working electrode is that metal electrode, reference electrode are goldBelong to silk, be sheet metal to electrode, three-electrode system reaction unit is connected with the wire of electrochemical workstation, start electrochemistryWork station, arranges automatic measurement parameter, waits for that measurement is complete, after measurement, data are derived, and by file name settingFor the form of " other-Celsius temperature-speed-other .txt ", wherein, " other " are the title of setting arbitrarily; " temperature CelsiusDegree " be the temperature of experiment, unit is DEG C; " speed " is the sweep speed of cyclic voltammetry curve, and unit is v/s.
2, described batch reads in file and specifically comprises: first data store organisation is set is four layer data structures,
Ground floor is data point p, corresponding current value and the potential value of each point on storage cyclic voltammetry curve;
The second layer is Data-Link dataInput, a Data-Link dataInput of each cyclic voltammetry curve composition, dataChain dataInput stores all data point p of this cyclic voltammetry curve;
The 3rd layer is data group dataGroup, and a data group dataGroup stores the number of temperature same loop volt-ampere curveAccording to, i.e. all dataInput Data-Links;
The 4th layer is dataAll structure, stores all dataGroup;
The relevant parameter of condition determination is set before reading data, comprises electrode area, reaction electron number and concentration, then input literary compositionPart folder position, searches the data files that meets naming rule all in given folder location, and is read in program, eachPoint p object of the electric current that every a line in individual txt file comprises and current potential Information generation, multiple in a txt fileP point object generates a dataInput Data-Link object, the temperature of existing dataGroup data group in audit program, asThe fruit wherein temperature of certain dataGroup data group is identical with the temperature of newly-generated dataInput, just by this dataInputDeposit this dataGroup data group in, if do not check the dataGroup identical with the temperature of newly-generated dataInput, justA newly-built dataGroup, in order to store this dataInput.
3, described in, carry out Data correction and pretreated method is: check one by one each Data-Link, by each point current value relatively,Potential value size is found out oxidation peak and reduction peak and p object corresponding to commutation potential point, then according to Nicholson formulaProofread and correct oxidation peak point current, then find point corresponding to reduction peak current half, for rearThe calculating of issue certificate.
The method of drawing 4, is:
(1) search current maxima and current minimum in each data group, determine current range; Search in each data groupCurrent potential maximum and potential minimum, determine potential range, wide and high according to required synthetic image, by current range divided by heightDetermine draw required ordinate ratio, then by potential range divided by the wide abscissa ratio that draws, then utilize vertical-horizontal proportion and electric currentThe relation of value potential value draws each point in image;
(2) search the subduplicate maximum of sweep speed and minimum of a value in each data group, determine the subduplicate model of sweep speedEnclose; Search current maxima and minimum of a value in each data group, determine current range, wide and high according to required synthetic image,Determine divided by height the required ordinate ratio of drawing by current value range, then by the subduplicate scope of sweep speed divided by the wide horizontal stroke that drawsCoordinate ratio, then utilizes vertical-horizontal proportion and current value, the subduplicate relation of sweep speed, and each point is drawn in image;
(3) search maximum and the minimum of a value of sweep speed logarithm value in each data group, determine the model of sweep speed logarithm valueEnclose; Search current potential maximum and minimum of a value in each data group, determine potential range, wide and high according to required synthetic image,Electricity consumption bit value ranges determines divided by height the required ordinate ratio of drawing, then by the scope of sweep speed logarithm value divided by the wide horizontal stroke that drawsCoordinate ratio, then utilizes the relation of vertical-horizontal proportion and potential value, sweep speed logarithm value, and each point is drawn in image.
5, described judgement reaction type specifically comprises:
(1) utilize calibrated oxidation peak and current value and the potential value of reduction peak to calculate, first, according to same temperatureReduction peak current under degree and the subduplicate data of sweep speed are carried out fitting a straight line, try to achieve straight slope, irreversible ifReaction, utilizes formulaCalculate D0; Reversible reaction if, utilizes formula Calculate D0；
(2) repeating step (1), calculates the D at all temperature0, according to LnD0Carry out fitting a straight line with 1/T data, obtainStraight slope, utilizes formula lnD=lnD0-Ea/ RT obtains reaction activity Ea；
(3) utilize formula ks＝2.18[D0(αnα)vF/RT]1/2exp[(Epc-Epa)α2NF/RT], often try to achieve reaction diffusionNumber ks。
In order to record easily electrochemical reaction parameters, the present invention uses cyclic voltammetry to combine with Automatic data processingScheme. The technology that wherein data are automatically processed realizes by cross-platform Java language, can independent process primary data, automaticallyCalculate response parameter, and can draw figure. Reduce greatly workload.
The main points of technical scheme of the present invention are embodied in:
Use three-electrode system reaction unit, by three electrode access electrochemical workstations, use cyclic voltammetry to measure initial numberAccording to. Re-use automatic data processing technique and calculate initial data, obtain final electrochemical reaction parameters and data relationship figure.
Automatic data processing technique is wherein used Java to programme as language. First the batch of, realizing file reads in. SoAfter, adopt the four layer data structures storages data of reading in, and from file name, read the information of temperature and sweep speed. AllAfter reading in and storing, carry out Data correction and pretreatment, and then draw according to the result after proofreading and correct, judge response classType, and obtain the data such as diffusion coefficient, reaction activity, speed constant in conjunction with computing formula. Finally demonstrate result of calculation withPicture.
The invention has the beneficial effects as follows:
Can record easily electrode reaction dynamics and thermodynamic parameter, greatly shorten determination period, reduce overall workload,Overall cost is cheap, and final calculation result can meet most of needs with the figure of drawing.
Brief description of the drawings
Fig. 1 is the flow chart of method of the present invention.
Fig. 2 is data structure diagram of the present invention.
Fig. 3 is the example I-E image that the present invention generates.
Fig. 4 is the example I-v that the present invention generates1/2Image.
Fig. 5 is the example E-logv image that the present invention generates.
Detailed description of the invention
For example the present invention is described in more detail below in conjunction with accompanying drawing.
(1) initial data measuring phases, as shown in Figure 1.The working electrode of three-electrode system reaction unit is metal electrode (as platinum disk electrode); Reference electrode be wire (asPlatinum filament); Be sheet metal (as platinized platinum) to electrode; Contain in addition a rotor, can accelerate by Electromagnetic DriveThe dissolving of reactant. First cleaning reaction device and associated components, guarantees that it is clean dry. Reactant is addedAfter reaction vessel, heat stirring and dissolving, until stable. Reaction unit is connected with the wire of electrochemical workstation,Start electrochemical workstation, automatic measurement parameter is set, wait for that measurement is complete. After measurement, data are ledGo out, and file name is set to the form of " other-Celsius temperature-speed-other .txt ". Wherein, " itsHe " be the title that user oneself sets arbitrarily; " Celsius temperature ", is the temperature of experiment, and unit is DEG C; " speedRate ", be the sweep speed of cyclic voltammetry curve, unit is v/s. Initial data can be used for calculating electrode reactionParameter.
(2) data input phase, as shown in Figure 1.
First data store organisation is set, and this method adopts four layer data structures, as shown in Figure 2.
1) ground floor is data point p, can store corresponding current value and the potential value of each point on cyclic voltammetry curve.
2) second layer is Data-Link dataInput, a Data-Link dataInput of each cyclic voltammetry curve composition,Article one, Data-Link dataInput stores all data point p of this cyclic voltammetry curve.
3) the 3rd layer is data group dataGroup, and a data group dataGroup stores temperature same loop volt-ampere songThe data of line, i.e. all dataInput Data-Links.
4) the 4th layer is dataAll structure, stores all dataGroup.
The relevant parameter of experiment condition is set before reading data, comprises electrode area, reaction electron number and concentration etc.Then import folders position, searches all meeting in given folder location and appeals the data literary composition of naming rulePart, and be read in program. The electric current that every a line in each txt file comprises and current potential Information generationA point p object, the multiple p point objects in a txt file generate a dataInput Data-Link object.The temperature of existing dataGroup data group in audit program, if certain dataGroup data group whereinTemperature is identical with the temperature of newly-generated dataInput, just this dataInput is deposited in to this dataGroup numberAccording to group. If do not check the dataGroup identical with the temperature of newly-generated dataInput, with regard to newly-built oneDataGroup, in order to store this dataInput.
In the process of reading in, will provide warning if there is mistake, show the title of error file.
(3) pretreatment stage, as shown in Figure 1.After reading in, start to carry out data pretreatment. Check one by one each Data-Link, by comparing each point current valuePotential value size is found out oxidation peak and reduction peak and p object corresponding to commutation potential point. Then basisNicholson formulaProofread and correct oxidation peak point current. Find again reduction peakThe point that electric current half is corresponding, for the calculating of later data.
(4) the synthetic image stage, as shown in Figure 1.
1) search current maxima and current minimum in each data group, determine current range; Search every numberAccording to current potential maximum and potential minimum in group, determine potential range. Wide and high according to required synthetic image,With current range divided by height determine draw required ordinate ratio, then by potential range divided by the wide abscissa ratio that drawsExample. Then the relation of utilizing vertical-horizontal proportion and current value potential value can draw each point in image. FinallyBe presented at appointed area. Fig. 3 is the I-E example image that this method generates.
2) search the subduplicate maximum of sweep speed and minimum of a value in each data group, determine sweep speed squareThe scope of root; Search current maxima and minimum of a value in each data group, determine current range. According to requiredSynthetic image wide and high, determines divided by height the required ordinate ratio of drawing by current value range, then with scanningThe subduplicate scope of speed is divided by the wide abscissa ratio that draws. Then utilize vertical-horizontal proportion and current value, scanning speedThe subduplicate relation of rate can draw each point in image. Finally be presented at appointed area. Fig. 4 is weThe I-v that method generates1/2Example image.
3) search maximum and the minimum of a value of sweep speed logarithm value in each data group, determine sweep speed logarithmThe scope of value; Search current potential maximum and minimum of a value in each data group, determine potential range. According to requiredSynthetic image wide and high, electricity consumption bit value ranges determines divided by height the required ordinate ratio of drawing, then with scanningThe scope of speed logarithm value is divided by the wide abscissa ratio that draws. Then utilize vertical-horizontal proportion and potential value, scanning speedThe relation of rate logarithm value can draw each point in image. Finally be presented at appointed area. Fig. 5 is weThe E-logv example image that method generates.
(5) judge reaction type and calculation stages, as shown in Figure 1.
1) judge reaction type according to Fig. 3, Fig. 4 and Fig. 5, select corresponding computational methods.
2) utilize calibrated oxidation peak and current value and the potential value of reduction peak to calculate. First, according to sameThe subduplicate data of the reduction peak current at temperature and sweep speed are carried out fitting a straight line, try to achieve straight slope.Irreversible reaction if, utilizes formula Can calculateD0; Reversible reaction if, utilizes formulaCan calculate D0。
3) repeat step above, calculate the D at all temperature0. According to LnD0Carry out fitting a straight line with 1/T data,Obtain straight slope. Utilize formula lnD=lnD0-Ea/ RT can obtain reaction activity Ea。
4), according to the data of above-mentioned calculating, utilize formula ks＝2.18[D0(anα)vF/RT]1/2exp[(Epc-Epa)α2NF/RT], can try to achieve reaction diffusion constant ks。
(6) result shows memory phase, as shown in Figure 1.After calculating, can show in territory, results display area diffusion coefficient D0, reaction activity Ea, rate constants ksEtc. data. Then can press from both sides by select File, the picture of current demonstration is existed to specified position.
Claims (2)
1. an assay method for electrode reaction parameter, by three electrode access electrochemical workstations of three-electrode system reaction unit,Use cyclic voltammetry to measure primary data, primary data is processed, obtain electrochemical reaction parameters and entity relationship diagramShape; It is characterized in that: described primary data is processed specifically and comprised: read in file first in batches, then adopt four layer dataThe data that structure storage is read in, and from file name, read the information of temperature and sweep speed, after all reading in and storing,Carry out Data correction and pretreatment, and then draw according to the result after proofreading and correct, judge reaction type, and in conjunction with computing formulaObtain diffusion coefficient, reaction activity, speed constant data, finally demonstrate result of calculation and picture;
Described three-electrode system is: working electrode is that metal electrode, reference electrode are wire, are sheet metal to electrode;
Described batch reads in file and specifically comprises: first data store organisation is set is four layer data structures,
Ground floor is data point p, corresponding current value and the potential value of each point on storage cyclic voltammetry curve;
The second layer is Data-Link dataInput, a Data-Link dataInput of each cyclic voltammetry curve composition, dataChain dataInput stores all data point p of this cyclic voltammetry curve;
The 3rd layer is data group dataGroup, and a data group dataGroup stores the number of temperature same loop volt-ampere curveAccording to, i.e. all dataInput Data-Links;
The 4th layer is dataAll structure, stores all dataGroup;
The relevant parameter of condition determination is set before reading data, comprises electrode area, reaction electron number and concentration, then input literary compositionPart folder position, searches the data files that meets naming rule all in given folder location, and is read in program, eachPoint p object of the electric current that every a line in individual txt file comprises and current potential Information generation, multiple in a txt fileP point object generates a dataInput Data-Link object, the temperature of existing dataGroup data group in audit program, asThe fruit wherein temperature of certain dataGroup data group is identical with the temperature of newly-generated dataInput, just by this dataInputDeposit this dataGroup data group in, if do not check the dataGroup identical with the temperature of newly-generated dataInput, justA newly-built dataGroup, in order to store this dataInput;
Describedly carry out Data correction and pretreated method is: check one by one each Data-Link, by each point current value relatively,Potential value size is found out oxidation peak and reduction peak and p object corresponding to commutation potential point, then according to Nicholson formulaProofread and correct oxidation peak point current, then find point corresponding to reduction peak current half, for rearThe calculating of issue certificate;
Described method of drawing is:
(1) search current maxima and current minimum in each data group, determine current range; Search in each data groupCurrent potential maximum and potential minimum, determine potential range, wide and high according to required synthetic image, by current range divided by heightDetermine draw required ordinate ratio, then by potential range divided by the wide abscissa ratio that draws, then utilize vertical-horizontal proportion and electric currentThe relation of value potential value draws each point in image;
(2) search the subduplicate maximum of sweep speed and minimum of a value in each data group, determine the subduplicate model of sweep speedEnclose; Search current maxima and minimum of a value in each data group, determine current range, wide and high according to required synthetic image,Determine divided by height the required ordinate ratio of drawing by current value range, then by the subduplicate scope of sweep speed divided by the wide horizontal stroke that drawsCoordinate ratio, then utilizes vertical-horizontal proportion and current value, the subduplicate relation of sweep speed, and each point is drawn in image;
(3) search maximum and the minimum of a value of sweep speed logarithm value in each data group, determine the model of sweep speed logarithm valueEnclose; Search current potential maximum and minimum of a value in each data group, determine potential range, wide and high according to required synthetic image,Electricity consumption bit value ranges determines divided by height the required ordinate ratio of drawing, then by the scope of sweep speed logarithm value divided by the wide horizontal stroke that drawsCoordinate ratio, then utilizes the relation of vertical-horizontal proportion and potential value, sweep speed logarithm value, and each point is drawn in image;
Described judgement reaction type specifically comprises:
(1) utilize calibrated oxidation peak and current value and the potential value of reduction peak to calculate, first, according to same temperatureReduction peak current under degree and the subduplicate data of sweep speed are carried out fitting a straight line, try to achieve straight slope, irreversible ifReaction, utilizes formulaCalculate D0; Reversible reaction if, utilizes formula Calculate D0；
(2) repeating step (1), calculates the D at all temperature0, according to LnD0Carry out fitting a straight line with 1/T data, obtainStraight slope, utilizes formula lnD=lnD0-Ea/ RT obtains reaction activity Ea；
(3) utilize formulaTry to achieve reaction diffusion normalNumber ks。
2. the assay method of electrode reaction parameter according to claim 1, is characterized in that described use cyclic voltammetry measurementGoing out primary data specifically comprises: three-electrode system reaction unit is connected with the wire of electrochemical workstation, starts electrochemistry workStand, automatic measurement parameter is set, wait for that measurement is complete, after measurement, data are derived, and file name is set toThe form of " other-Celsius temperature-speed-other .txt ", wherein, " other " are the title of setting arbitrarily; " Celsius temperature "For the temperature of experiment, unit is DEG C; " speed " is the sweep speed of cyclic voltammetry curve, and unit is v/s.
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