Summary of the invention
In order to solve above-mentioned deficiency of the prior art, the invention provides a kind of electrode surface processing method and device that is applied in the electrochemistry.
For achieving the above object, the present invention adopts following technical scheme:
A kind of electrode surface processing method may further comprise the steps:
A, utilize the clamp mechanism fixed electrode, make electrode perpendicular to the polishing cloth that is arranged on the rotating disk;
Put polishing powder to polishing cloth and add solvent, make polishing powder and solvent form emulsion;
B, clamp mechanism is exerted pressure with the pressure between control electrode and the polishing cloth, rotate rotating disk, electrode surface is polished until reaching requirement.
Further, described electrode is the inconsistent double-decker of ectonexine material.
Further, rotary speed is not more than 200r/min.
Further, the pressure that is applied on the clamp mechanism is not more than 50N.
Further, in step b, the polishing electrode time is not more than 300s.
As preferably, in step b, adopt pressing mechanism that clamp mechanism is exerted pressure.
As preferably, the adopts pressure sensor measurement is applied to the pressure on the clamp mechanism, and FEEDBACK CONTROL is applied to pressure on the clamp mechanism in view of the above.
The present invention also provides a kind of treatment of electrode surfaces device, comprises polishing mechanism, clamp mechanism, actuating unit and bearing; Described polishing mechanism, clamp mechanism link to each other with bearing respectively;
Described polishing mechanism comprises rotating disk and polishing cloth, and described polishing cloth is arranged on the rotating disk;
Described clamp mechanism is arranged on the top of polishing mechanism; Described clamp mechanism fixed electrode makes electrode perpendicular to the polishing cloth that is arranged on the rotating disk, and bears pressure, and electrode is contacted with polishing cloth;
Described actuating unit control dial rotation.
Further, described electrode is the inconsistent double-decker of ectonexine material.
As preferably, described treating apparatus also comprises the pressure sensor that is arranged on the clamp mechanism, measures the pressure that is applied on the clamp mechanism.
Described treating apparatus also comprises pressing mechanism, and described pressing mechanism is arranged on the top of bearing upper clamping mechanism, and contacts with it.
Further, described treating apparatus also comprises respectively the pressure feedback module that links to each other with pressure sensor with pressing mechanism, is applied to pressure on the clamp mechanism with the control pressue device.
As preferably, described clamp mechanism is screw lock or snap locking or electromagnetic locking structure.
The present invention compared with prior art has following beneficial effect:
1, adopt mechanical device directly electrode surface to be polished, and polishing effect is good, exploitativeness is strong, can realize general electrode surface polishing; The defective of having avoided effect hand-manipulated to guarantee;
2, having avoided electrode to handle needs the specialized skills problem, makes the personnel that do not have electrochemistry specialty background can carry out polishing electrode and handles;
3,, avoided electrode is directly exerted pressure and caused the damage of electrode structure by clamp mechanism is exerted pressure with the pressure between control electrode and the polishing cloth;
4, because need not artificial hand steered electrode, just greatly alleviated the graininess polishing powder to the infringement that human body causes, improved electrode Processing Test operating environment;
Rotary speed can be adjusted during 5, owing to polishing electrode, can realize the treatment of electrode surfaces problems such as disc electrode to inside and outside two layers of material differs, physical property differs greatly under the less situation of rotary speed;
6, the polishing electrode parameter is limited, so that electrode is under suitable rotating speed and pressure condition, the polishing certain hour, obtain comparatively satisfied polishing effect, avoided the electrode phenomenon of leakage that brings because of rotating speed is excessive, also avoided crossing the waste that ambassador's wear to electrodes too much brings electrode because of pressure;
7, saved the electrode processing time, reduced simultaneously because the relatively poor possibility of test effect that electrode is handled problems and caused.
The specific embodiment
Of the present invention vertically is not absolute vertical, allows to exist certain error when satisfying the electrode processing requirements.
Embodiment 1
See also Fig. 2 and Fig. 3, a kind of treatment of electrode surfaces device comprises polishing mechanism 1, clamp mechanism 21, actuating unit 4 and bearing 5;
Described polishing mechanism 1, clamp mechanism 21 link to each other with base 5 respectively;
Described polishing mechanism 1 comprises rotating disk 11 and polishing cloth 12, and described polishing cloth 12 is fixed on the rotating disk 11, and described polishing cloth 12 is chamois leather or abrasive paper for metallograph, and present embodiment adopts chamois leather;
Described clamp mechanism 21 is arranged on the top of polishing mechanism 1;
See also Fig. 4, Fig. 5 and Fig. 6, described clamp mechanism 21 comprises backboard 211, pressing plate 212, locking mechanism and guide rail 214, and described locking mechanism is snap 213 and handle 216;
Relative position at described backboard 211 and pressing plate 212 is provided with groove 215, is used to place electrode 10, and guarantees that electrode 10 is perpendicular to the polishing cloth 12 that is arranged on the rotating disk 11;
Described backboard 211 and pressing plate 212 adopt snap 213 lockings, be used to adjust distance between backboard 211 and the pressing plate 212 with fixed electrode 10, guarantee simultaneously that electrode 10 can not be offset when electrode 10 fully contacts and rotates 11 pairs of electrodes 10 of rotating disk and polishes with polishing cloth 12, inclination etc.;
See also Fig. 7, the top of described clamp mechanism 21 also is provided with compression module, and described compression module comprises forcing screw 311 and head 312;
Described head 312 bottoms closely contact with clamp mechanism 21, and a medium altitude groove 314 is arranged at head 312 bottoms, so that electrode 10 first halves can be deep enough to head 312 inside, and it is contactless between electrode 10 upper surfaces and the head 312 internal recess surfaces, when head 312 being exerted pressure with assurance, head 312 only passes to pressure clamp mechanism 21, and can not destroy the structure of electrode 10; Forcing screw 311 directly contacts with head 312, makes the pressure that is applied on the forcing screw 311 can be directly passed to head 312, and further passes to clamp mechanism 21;
When clamp mechanism 21 was exerted pressure, impetus was directly avoided the position of electrode on clamp mechanism, also can be on the forcing screw 311 of compression module, also by head 312 transmission pressure; As long as can exert pressure, directly electrode is not applied power again simultaneously and get final product clamp mechanism 312; Present embodiment is to be provided with compression module, manually by compression module power is applied on the clamp mechanism 21;
Described clamp mechanism 21 can be along guide rail 214 translations when being subjected to external force, and electrode 10 is fully contacted with the polishing cloth 12 of polishing mechanism 1;
Described actuating unit 4 control rotating disks 11 rotate.
Present embodiment also provides a kind of electrode surface processing method, may further comprise the steps:
A, provide present embodiment described treatment of electrode surfaces device;
Rotary handle 216, snap 213 flicks, and raises pressing plate 212, and glass carbon disk electrode 10 is put into groove 215 between backboard 211 and the pressing plate 212, to guarantee that electrode 10 is perpendicular to the polishing cloth 12 that is arranged on the described rotating disk 11; Pressing plate 212 is closed up, and snap 213 pins and fixed electrode 10, utilizes the snap 213 automatic distances of adjusting between backboard 241 and the pressing plate 242;
Polishing powder is put near polishing cloth 12 top electrodes 10 polished surface, added solvent, make polishing powder and solvent form emulsion; Described polishing powder is that particle diameter is the alumina particle of 0.05 μ m; Described solvent is the mixture of water or water and ethanol, and present embodiment is selected water for use;
B, manually live forcing screw 311 with hand and it is exerted pressure, pressure passes to clamp mechanism 21 through head 312; Because electrode 10 is fixed on the 21 inner also whiles of clamp mechanism and contacts with polishing cloth 12, then can change paired electrode 10 applied pressures to clamp mechanism 21 applied pressures, thereby increase the pressure between electrode 10 and the polishing cloth 12, and then increase the frictional force between the electrode 10 and polishing cloth 12 when rotating disk 11 rotates, thereby effectively electrode 10 is polished; Avoided directly damage that electrode 10 is exerted pressure and may be brought electrode 10 simultaneously;
Rule of thumb control is applied to the size of the pressure on the clamp mechanism 21, generally is controlled at 10N;
It is n=20r/min that rotating disk 11 rotating speeds are set; Rotate rotating disk 11, electrode 10 surfaces are polished; Rule of thumb to stopping behind the electrode 10 polishing 300s.
In the polishing electrode process, less rotating speed makes electrode less because of the distortion that frictional heat produces, and makes that polishing to electrode is easier to reach requirement.
Embodiment 2
See also Fig. 8, a kind of treatment of electrode surfaces device, different with embodiment 1 described treatment of electrode surfaces device is: described treating apparatus also comprises pressure sensor 313, and described pressure sensor 313 is arranged between forcing screw 311 and the head 312.
Present embodiment also provides a kind of electrode surface processing method, and different with embodiment 1 described electrode surface processing method is:
In step a, provide present embodiment described treatment of electrode surfaces device;
In step b, pressure sensor 313 is measured in real time manually with hand and is applied to pressure on the forcing screw 311, and adjusts by the force value that pressure sensor 313 shows, so that pressure remains on 15N substantially, error is controlled at ± 0.5N;
It is n=50r/min that rotating disk 11 rotating speeds are set; Rotate rotating disk 11, electrode 10 surfaces are polished; Rule of thumb to stopping behind the electrode 10 polishing 200s.
Embodiment 3
Please refer to Fig. 9, Figure 10, a kind of treatment of electrode surfaces device, different with embodiment 2 described treatment of electrode surfaces devices is:
The locking mechanism of clamp mechanism is screw 233 and spanner, and spanner is not shown in the diagram; At backboard 231 and pressing plate 232 relative positions groove 235 is set, is used to place electrode 10, and guarantee that electrode 10 is perpendicular to the polishing cloth 12 that is arranged on the rotating disk 11; Described backboard 231 and pressing plate 232 adopt screw 233 lockings, be used to adjust distance between backboard 231 and the pressing plate 232 with fixed electrode 10, guarantee simultaneously that electrode 10 can not be offset when electrode 10 fully contacts and rotates 11 pairs of electrodes 10 of rotating disk and polishes with polishing cloth 12, inclination etc.; Clamp mechanism can be along guide rail 214 translations when being subjected to external force.
Present embodiment also provides a kind of electrode surface processing method, and different with embodiment 2 described electrode surface processing methods is:
In step a, provide present embodiment described treatment of electrode surfaces device;
Glass carbon disk electrode 10 is put into groove 235 between backboard 231 and the pressing plate 232, screw screw 233 with described spanner, perpendicular to the polishing cloth 12 that is arranged on the described rotating disk 11, adjust distance and fixed electrode 10 between backboard 231 and the pressing plate 232 to guarantee electrode 10 simultaneously;
In step b, pressure sensor 313 is measured in real time manually with hand and is applied to pressure on the forcing screw 311, and adjusts people's hand-power in real time by the force value that pressure sensor 313 shows, so that pressure remains on 20N substantially, error is controlled at ± 0.3N;
It is n=80r/min that rotary speed is set; Rule of thumb to stopping behind the polishing electrode 150s.
Embodiment 4
Please refer to Figure 11, Figure 12, a kind of treatment of electrode surfaces device, different with embodiment 2 described treatment of electrode surfaces devices is:
The locking mechanism of clamp mechanism is an electromagnetic plate, and backboard 241 and pressing plate 242 adopts electromagnetic lockings, is used to adjust distance between backboard 241 and the pressing plate 242 with fixed electrode 10; Described backboard 241 and pressing plate 242 materials are magnetic sheet, and magnetic sheet phase energy-absorbing is enough in backboard 241 and pressing plate 242 lockings.
Present embodiment also provides a kind of electrode surface processing method, and different with embodiment 2 described electrode surface processing methods is:
In step a, provide present embodiment described treatment of electrode surfaces device;
Electrode is put into groove 245 between backboard 241 and the pressing plate 242, to guarantee that electrode 10 is perpendicular to the polishing cloth 12 that is arranged on the described rotating disk 11; Pressing plate 242 is closed up, and backboard 241 and pressing plate 242 electromagnetism are inhaled electrode 10 fixing mutually, utilize electromagnetism to inhale distance between automatic adjustment backboard 241 and the pressing plate 242 mutually;
In step b, pressure sensor 313 is measured in real time manually with hand and is applied to pressure on the forcing screw 311, and adjusts people's hand-power in real time by the force value that pressure sensor 313 shows, so that pressure remains on 30N substantially, error is controlled at ± 1N;
It is n=60r/min that rotary speed is set; To stopping behind the polishing electrode 120s.
Embodiment 5
See also Figure 13, Figure 14, a kind of treatment of electrode surfaces device, different with embodiment 1 described treatment of electrode surfaces device is: described treating apparatus also comprises pressing mechanism, pressure sensor and pressure feedback module;
Described pressing mechanism 35 is arranged on the top of clamp mechanism 25 and clamp mechanism 25 is exerted pressure;
Described pressing mechanism 35 comprises actuator 351, driving member 352 and briquetting 353;
The driving voltage control actuator 351 of power supply output drives driving member 352 and promotes briquetting 353, can realize the object that contacts with briquetting 353 is exerted pressure; In the present embodiment, the actuator 351 in the pressing mechanism 35 is a motor, and driving member 352 is a screw mandrel, and according to the control of electric power output voltage, the driven by motor screw mandrel promotes 353 pairs of clamp mechanism 25 of briquetting and exerts pressure;
Briquetting 353 can directly replace the compression module among the embodiment 1, and its elongated portion is linked to each other with screw mandrel; In this case, the bottom of described briquetting 353 closely contacts with clamp mechanism 25, and briquetting 353 bottoms and the contacted one side of clamp mechanism have a medium altitude groove, so that electrode 10 first halves can be deep enough to briquetting 353 inside, and it is contactless between electrode 10 upper surfaces and the briquetting 353 internal recess surfaces, when with assurance briquetting 353 being exerted pressure, briquetting 353 only passes to pressure clamp mechanism 25, and can not destroy the structure of electrode 10;
Briquetting 353 also can be arranged on the top of compression module, directly the forcing screw of compression module is exerted pressure, and by head power is passed to clamp mechanism 25;
In the present embodiment, briquetting 353 is arranged on the top of compression module;
Described pressure sensor is arranged between briquetting 353 and the head, measures the pressure that is applied on the clamp mechanism 25;
Described pressure feedback module links to each other with the power supply of pressure sensor with actuator 351 respectively, output with force value FEEDBACK CONTROL actuator 351 power supplys that record according to pressure sensor, be applied to pressure on the electrode with control, so that the electrode applied pressure is stabilized in certain error range.
Present embodiment also provides a kind of electrode surface processing method, and different with embodiment 1 described electrode surface processing method is:
In step a, electrode structure is inside and outside two-layer, and inner layer material is glass carbon, gold or platinum, and skin is polytetrafluoroethylene (PTFE) or polyether-ether-ketone resin (PEEK); The characteristics of this structure are that internal layer and outer hardness and other physical property differ greatly; The electrode inner layer material is a glass carbon in the present embodiment, and skin is a polytetrafluoroethylene (PTFE);
Provide present embodiment described treatment of electrode surfaces device;
In step b, it is n=150r/min that rotary speed is set, and it is 30N that 35 pairs of clamp mechanism 2 applied pressures of pressing mechanism are set, and it is 100s that rotating disk 11 rotation times are set;
Rotate rotating disk 11,35 pairs of electrodes of pressing mechanism are exerted pressure, the described pressure of while pressure sensor monitoring, and by the described pressure of pressure feedback module controls, to guarantee that the pressure perseverance that is applied on the clamp mechanism 25 is 30N; Electrode surface is polished, stop behind the 100s;
Originally executing the routine pressing mechanism that is adopted is closed loop feedback system, after receiving instruction, the driven by motor screw mandrel of pressing mechanism 35 promotes 2 pressurizations of 353 pairs of clamp mechanism of briquetting, pressure sensor monitoring is applied to the pressure on the clamp mechanism 2, the motor of the force value FEEDBACK CONTROL pressing mechanism 35 that the pressure feedback module records according to pressure sensor, and then the control briquetting is applied to the pressure on the clamp mechanism 2, the error that guarantees pressure simultaneously is controlled at ± 0.1N, by the precision that guarantees polishing that is provided with, thereby realize full automatic polishing to polishing time;
Because the electrode surface structure there are differences, when polishing, less rotating speed can make electrode surface each several part polishing velocity more consistent, realizes the purpose of electrode surface polishing simultaneously, has been avoided electrode " leakage " phenomenon.
Take out electrode, clean 3 times with clear water, it is residual that electrode surface does not have obvious polishing material;
Utilize cyclic voltammetry that electrode surface is measured, whether reach requirement with the inspecting electrode surface finish:
For reversible system, when adopting cyclic voltammetry scanning, oxidation peak current potential and reduction peak current potential difference have following formula:
Wherein:
Be the oxidation peak current potential,
Be the reduction peak current potential, electronics transmitted number when n was reversible reaction;
Simultaneously, according to Landells-Xiu Wei odd-numbered prescription journey (Randles-Sevcik), oxidation peak current and reduction peak current have following formula:
Wherein, i
PaBe oxidation peak current potential, i
PcBe the reduction peak current potential.
According to above theory, select the reversible reaction system potassium ferricyanide [K
3Fe (CN)
6] carry out the judgement of electrode availability; Under this system, if polishing electrode is satisfactory for result, oxidation peak and reduction peak current potential differ 56mV under the theoretical case, oxidation peak current and reduction peak current ratio are 1, consider the reagent situation, oxidation peak current potential and reduction peak current potential difference are below the 80mV, and oxidation peak and reduction peak current difference are 0.9-1.1, think that promptly electrode can use; If do not reach this condition, need to continue electrode is carried out polishing;
Present embodiment adopts K3Fe (CN) 6 (the NaCl solution that includes 0.20mol/L is as the supporting electrolyte) solution of 0.0005mol/L to carry out the check of electrode availability; During check, adopt occasion China CHI650C electrochemical workstation, auxiliary electrode is the Pt electrode, and reference electrode is Ag/AgCl (3mol/LKCl) electrode; It is as follows that cyclic voltammetry is provided with parameter: onset potential-0.2V, high level 0.6V, low level-0.2V, sweep speed 50mV/s; With before the polishing of described glass carbon disk electrode and after carry out cyclic voltammetry sweep waveform under the same terms respectively as Figure 15, shown in Figure 16; Can learn by analyzing:
Before polishing electrode, the oxidation peak current potential is 0.230V, and oxidation peak electricity electric current is-1.010e-5A, the reduction peak current potential is 0.353V, reduction peak current is-1.052e-5A, and oxidation peak and reduction peak current potential difference are 124mV, and oxidation peak current and reduction peak current ratio are 0.96;
After polishing electrode, the oxidation peak current potential is 0.257V, and oxidation peak electricity electric current is-1.330e-5A, the reduction peak current potential is 0.326V, reduction peak current is-1.387e-5A, and oxidation peak and reduction peak current potential difference are 69mV, and oxidation peak current and reduction peak current ratio are 0.96;
Compare before the polishing electrode and effect afterwards, as can be seen: oxidation peak and reduction peak current potential difference are 124mV before the polishing, and big gap are arranged below the criterion 80mV, and polish the rear oxidation peak and reduction peak current potential difference is 69mV, meet described criterion, therefore polishing effectively.
Because rotary speed can be adjusted during polishing electrode, can under the less situation of rotary speed, realize treatment of electrode surfaces problems such as disc electrode to inside and outside two layers of material differs, physical property differs greatly;
Simultaneously, saved the electrode processing time, reduced because the relatively poor possibility of test effect that electrode is handled problems and caused;
Present embodiment is breaking away under the artificial situation fully, has realized the polishing to electrode surface, makes the personnel that do not have electrochemistry specialty background also can carry out polishing electrode and handles; Improved electrode Processing Test operating environment simultaneously.
Embodiment 6
A kind of treatment of electrode surfaces device is identical with embodiment 5 described treatment of electrode surfaces devices.
Present embodiment also provides a kind of electrode surface processing method, and different with embodiment 5 described electrode surface processing methods is:
In step b, it is n=180r/min that rotary speed is set, and it is 40N that 35 pairs of clamp mechanism 25 applied pressures of pressing mechanism are set, and it is 80s that rotating disk 11 rotation times are set; After the polishing electrode, take out electrode, clean 3 times with clear water, it is residual that electrode surface does not have obvious polishing material;
Adopt cyclic voltammetry that electrode is carried out the availability check, as Figure 17, shown in Figure 180; Can learn by analyzing:
Before polishing electrode,, can't seek out peak because electrode performance is relatively poor;
After polishing electrode, the oxidation peak current potential is 0.254V, and oxidation peak electricity electric current is-1.273e-5A, the reduction peak current potential is 0.325V, reduction peak current is-1.361e-5A, and oxidation peak and reduction peak current potential difference are 71mV, and oxidation peak current and reduction peak current ratio are 0.94;
Relatively before the polishing electrode and effect afterwards, as can be seen: electrode performance is too poor before the polishing, can't seek out oxidation peak and reduction peak position, and polishing rear oxidation peak is 71mV with reduction peak current potential difference, meets described criterion, and therefore polishing is effective.
Embodiment 7
A kind of treatment of electrode surfaces device is identical with embodiment 5 described treatment of electrode surfaces devices.
Present embodiment also provides a kind of electrode surface processing method, and different with embodiment 5 described electrode surface processing methods is:
In step b, it is n=100r/min that rotary speed is set, and it is 50N that 35 pairs of clamp mechanism 25 applied pressures of pressing mechanism are set, and it is 50s that rotating disk 11 rotation times are set; After the polishing electrode, take out electrode, clean 3 times with clear water, it is residual that electrode surface does not have obvious polishing material;
Adopt cyclic voltammetry that electrode is carried out the availability check, as Figure 19, shown in Figure 20; Can learn by analyzing:
Before polishing electrode, the oxidation peak current potential is 0.196V, and oxidation peak electricity electric current is-20417e-5A, the reduction peak current potential is 0.364V, reduction peak current is-2.317e-5A, and oxidation peak and reduction peak current potential difference are 168mV, and oxidation peak current and reduction peak current ratio are 0.96;
After polishing electrode, the oxidation peak current potential is 0.248V, and oxidation peak electricity electric current is-3.376e-5A, the reduction peak current potential is 0.318V, reduction peak current is-3.437e-5A, and oxidation peak and reduction peak current potential difference are 71mV, and oxidation peak current and reduction peak current ratio are 0.98;
Compare before the polishing electrode and effect afterwards, as can be seen: oxidation peak and reduction peak current potential difference are 168mV before the polishing, with big gap is arranged below the criterion 80mV, and polishing rear oxidation peak and reduction peak current potential difference are 71mV, meet described criterion, oxidation wind and reduction peak current ratio also more approach theoretical value, and therefore polishing effectively.
Embodiment 8
A kind of treatment of electrode surfaces device is identical with embodiment 5 described treatment of electrode surfaces devices.
Present embodiment also provides a kind of electrode surface processing method, and different with embodiment 5 described electrode surface processing methods is:
In step b, it is n=200r/min that rotary speed is set, and it is 25N that setting adds 35 pairs of clamp mechanism 25 applied pressures of mechanism, and it is 30s that rotating disk 11 rotation times are set; After the polishing electrode, take out electrode, clean 3 times with clear water, it is residual that electrode surface does not have obvious polishing material;
Adopt cyclic voltammetry that electrode is carried out the availability check, as Figure 21, shown in Figure 22; Can learn by analyzing:
Before polishing electrode,, can't seek out peak because electrode performance is relatively poor;
After polishing electrode, the oxidation peak current potential is 0.254V, and oxidation peak electricity electric current is-1.828-5A, the reduction peak current potential is 0.314V, reduction peak current is-1.847e-5A, and oxidation peak and reduction peak current potential difference are 60mV, and oxidation peak current and reduction peak current ratio are 0.99;
Relatively before the polishing electrode and effect afterwards, as can be seen: electrode performance is too poor before the polishing, can't seek out oxidation peak and reduction peak position, and polishing rear oxidation peak is 60mV with reduction peak current potential difference, meets described criterion, and therefore polishing is effective.
Above-mentioned embodiment should not be construed as limiting the scope of the invention.Key of the present invention is: utilize the clamp mechanism fixed electrode and make electrode and polishing cloth perpendicular, realize the electrode especially automatic polishing of the inconsistent electrode surface of ectonexine framework by the pressure between control electrode and the polishing cloth and rotating speed simultaneously.Under the situation that does not break away from spirit of the present invention, any type of change that the present invention is made all should fall within protection scope of the present invention.