CN103293204A - Preparation method of iridium oxide microelectrode controlling electrochemical property by using activated circulation - Google Patents
Preparation method of iridium oxide microelectrode controlling electrochemical property by using activated circulation Download PDFInfo
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Abstract
The invention provides a preparation method of an iridium oxide microelectrode controlling an electrochemical property by using activated circulation. In the method, an iridium microelectrode array obtained by using sputtering is electrochemically activated into iridium oxide; a working electrolyte is normal saline; an activation method is that the voltage of a working electrode is scanned within a range from -1V to +1V; the scanning speed is 100mV/s; one circulating time is finished by scanning for one time. The preparation method disclosed by the invention is simple and convenient in operation and can strictly control the electrochemical property of the iridium oxide microelectrode array; the electrochemical property of the microelectrode can strictly controlled according to an obtained quantitative relation; with regard to in-situ activation or reactivation, the fewest activation times can be used for realizing the needed electrochemical property and the additional damages caused by the activation are reduced.
Description
Technical field
The present invention relates to a kind of microelectrode array of medical equipment technical field, particularly, relate to a kind of preparation method by the yttrium oxide microelectrode that activates the cycle control electrochemical properties.
Background technology
In recent years, along with MEMS (micro electro mechanical system) (MEMS:Micro-Electro-Mechanical Systems) continuous advancement in technology, make micro-system ranges of application such as microelectronic device and microsensor constantly enlarge, be widely used in a plurality of fields, particularly medical domain.
Microelectrode by the preparation of materials such as noble metal platinum, gold and iridium is to utilize micro electro mechanical system (MEMS) technology to use a typical case of biomedical aspect.Based on iridium, obtain the method for yttrium oxide by electrochemical method, the equipment, the method that need are simple, have obtained the attention of Many researchers.But the character of the yttrium oxide that is activated by electrochemical method and the strict quantitative relationship of Activiation method are not then received attention.
China's application number 200710052206.9, application publication number CN101057780 discloses a kind of iridium oxide electrode and manufacture method thereof in this patent.Described electrode is specially adapted to neuroelectricity record and neural micro-electrical stimulation, and the pH sensor.Iridium oxide electrode of the present invention has an insulation course, wherein encapsulates an electrode cores at least; Described electrode cores is that an at least one end is to have reactivation on the metal iridium bottom to generate the electric conductor on yttrium oxide top layer in metal iridium or non-iridium metals outside deposition, and the one end is connected with lead, and the yttrium oxide top layer exposes outside insulation course.Kind electrode is obtained by the iridium metals silk, and galvanochemistry activates and the control method of yttrium oxide character but all do not provide in this patent and the prior art.So, in actual use, should use and be subjected to more restriction.
To sum up, though the preparation method of the yttrium oxide microelectrode array that galvanochemistry activates has obtained certain research, but the character of the yttrium oxide that the electrochemical method that do not appear in the newspapers in the document activates and the control device of Activiation method, therefore, the invention provides a kind of preparation method of yttrium oxide microelectrode, address this problem.
Summary of the invention
At defective of the prior art, the purpose of this invention is to provide a kind of preparation method by the yttrium oxide microelectrode that activates the cycle control electrochemical properties, easy and simple to handle, can the strict electrochemical properties of controlling the yttrium oxide microelectrode array.And the character of the yttrium oxide that can activate by electrochemical method and the control of Activiation method concern that original position reactivates yttrium oxide.
For achieving the above object, the invention provides a kind of preparation method by the yttrium oxide microelectrode that activates the cycle control electrochemical properties, the iridium microelectrode array galvanochemistry that described method utilizes sputter to obtain activates and is yttrium oxide, working electrolyte is physiological saline, Activiation method is working electrode voltage at-1V to+1V scanning, sweep velocity is 100mV/s(millivolt per second), run-down is a cycle index.
Preferably, the concrete preparation process of described iridium microelectrode array is as follows:
At first get rid of the positive glue of 5 μ m and graphical at the Si sheet, the sputtered titanium Seed Layer, the 100-1000 dust, splash-proofing sputtering metal iridium 300 nanometers adopt Lift-off technology to remove photoresist again, graphical Seed Layer and iridium metals layer formation electrode;
And then deposit the Parylene-C of 5 μ m, and for the second time graphical photoresist, use reactive ion etching (RIE) that Parylene-C is carved and wear, expose electrode points, formation microelectrode array overlayer; So just prepared the iridium microelectrode array;
Before next step carried out galvanochemistry activation yttrium oxide microelectrode array, the iridium microelectrode array must pass through 10 minutes the ultrasonic cleaning respectively of acetone, alcohol, deionized water.
Preferably, the concrete galvanochemistry Activiation method of described galvanochemistry activation yttrium oxide microelectrode array is as follows:
The working electrolyte that galvanochemistry activates is physiological saline, and Activiation method is working electrode voltage at-1V to+1V scanning, and sweep velocity is 100mV/s(millivolt per second), run-down is a cycle index, namely 20 seconds is the time of a circulation; Contrast electrode is the Ag/AgCl electrode, is the platinized platinum electrode to electrode.
Preferably, the scope of charge storage before and after galvanochemistry activates of the described yttrium oxide microelectrode that is activated by galvanochemistry is 1.69-40.07mC/cm
2
Preferably, the charge storage of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=0.08615x+1.9873 in the control method that 100 times of beginning activate in the circulation, and x is cycle index, and y is charge storage.
Preferably, the charge storage of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=0.07792x+3.082 in the control method that activates in the circulation for the 100th time to the 200th time, and x is cycle index, and y is charge storage.
Preferably, the charge storage of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=0.07439x+3.298 in the control method that activates in the circulation for the 200th time to the 500th time, and x is cycle index, and y is charge storage.
Preferably, the control method of the redox peak separation of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=0.6541+0.00189x-8.875 * 10
-6x
2+ 2.1126 * 10
-8x
3-1.827 * 10
-11x
4, x is cycle index, y is the redox peak separation.
Preferably, the control method of the 1kHz impedance magnitude of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=-3291 * 0.9790
x+ 4321, y is the 1kHz impedance magnitude.
Preferably, the control method of the 1kHz impedance angle of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=-8.609-59.57 * 0.9611
x, y is the 1kHz impedance angle.
Preferably, the control method of the electric double layer capacitance of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=2.962 * 10
-9X+6.531 * 10
-8, x is cycle index, y is electric double layer capacitance.
Preferably, the control method of the capacitive maximum point of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=-87.10+11.24 * 0.9487
x, x is cycle index, y is the capacitive maximum point.
Preferably, the control method of the resistive maximum point of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=-6.629-16.22 * 0.9842
x, x is cycle index, y is resistive maximum point.
Compared with prior art, the present invention has following beneficial effect:
Preparation method of the present invention utilizes the character of the yttrium oxide that the iridium microelectrode array of micro-processing technology preparation, electrochemical method activate and the strict quantitative relationship of Activiation method.The present invention is easy and simple to handle, electrochemical properties that can strict control yttrium oxide microelectrode array; Can be according to the electrochemical properties of the strict control of the quantitative relationship that obtains microelectrode; Activate or activate again for original position, can use minimum activation number of times to realize the electrochemical properties that needs, reduce and activate the additional injury that produces.
Description of drawings
By reading the detailed description of non-limiting example being done with reference to the following drawings, it is more obvious that other features, objects and advantages of the present invention will become:
Fig. 1 is the SEM photo of one embodiment of the invention iridium microelectrode electrode points;
Fig. 2 is that one embodiment of the invention activates the current-time curvel that circulates preceding 55 times;
Fig. 3 is the current-time curvel that one embodiment of the invention activates circulation for the 55-100 time;
Fig. 4 is the current-time curvel that one embodiment of the invention activates circulation for the 100-500 time;
Fig. 5 is the variation of valence process of iridium in one embodiment of the invention activation;
Fig. 6 is the SEM photo of the yttrium oxide film of one embodiment of the invention iridium film, galvanochemistry activation;
Fig. 7 is that one embodiment of the invention activates the CV curve that circulates preceding 100 times;
Fig. 8 is one embodiment of the invention microelectrode charge storage and activates the graph of a relation that circulates preceding 100 times;
Fig. 9 is the CV curve that one embodiment of the invention activates circulation for the 100-500 time;
Figure 10 is the graph of a relation that one embodiment of the invention microelectrode charge storage and the 100-500 time activate circulation;
Figure 11 is one embodiment of the invention redox peak separation and the graph of a relation that activates cycle index;
Figure 12 is that one embodiment of the invention activates the impedance magnitude curve that circulates preceding 100 times;
Figure 13 is the impedance magnitude curve that one embodiment of the invention activates circulation for the 100-500 time;
Figure 14 is one embodiment of the invention 1kHz impedance magnitude and the graph of a relation that activates cycle index;
Figure 15 is one embodiment of the invention electric double layer capacitance and the graph of a relation that activates cycle index;
Figure 16 is that one embodiment of the invention activates the impedance angle curve that circulates preceding 100 times;
Figure 17 is the impedance angle curve that one embodiment of the invention activates circulation for the 100-500 time;
Figure 18 is one embodiment of the invention 1kHz impedance angle and the graph of a relation that activates cycle index;
Figure 19 is one embodiment of the invention capacitive maximum point and resistive maximum point and the graph of a relation that activates cycle index.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.Following examples will help those skilled in the art further to understand the present invention, but not limit the present invention in any form.Should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
The preparation method of the described yttrium oxide microelectrode that is activated by galvanochemistry utilizes the character of the yttrium oxide that the iridium microelectrode array of micro-processing technology preparation, electrochemical method activate and the strict quantitative relationship of Activiation method, described strict quantitative relationship is in physiological saline, working electrode voltage obtains to+1V scanning at-1V, and run-down is a cycle index.
The concrete preparation process of described iridium microelectrode array is as follows:
At first get rid of the positive glue of 5 μ m and graphical at the Si sheet, the sputtered titanium Seed Layer, the 100-1000 dust, splash-proofing sputtering metal iridium 300 nanometers adopt Lift-off technology to remove photoresist again, graphical Seed Layer and iridium metals layer formation electrode;
And then deposit the Parylene-C of 5 μ m, and for the second time graphical photoresist, use reactive ion etching (RIE) that Parylene-C is carved and wear, expose electrode points, formation microelectrode array overlayer; So just prepared the iridium microelectrode array;
Before next step carried out galvanochemistry activation yttrium oxide microelectrode array, the iridium microelectrode array must pass through 10 minutes the ultrasonic cleaning respectively of acetone, alcohol, deionized water.
The concrete galvanochemistry Activiation method of described galvanochemistry activation yttrium oxide microelectrode array is as follows:
The working electrolyte that galvanochemistry activates is physiological saline, and Activiation method is working electrode voltage at-1V to+1V scanning, and sweep velocity is 100mV/s(millivolt per second), run-down is a cycle index, namely 20 seconds is the time of a circulation; Contrast electrode is the Ag/AgCl electrode, is large-area platinized platinum electrode to electrode.
As shown in Figure 1, be the SEM photo of present embodiment iridium microelectrode electrode points: the diameter of electrode points is 100 microns, and this is to use size in typical electrode points of electric physiology application, and the iridium of present embodiment is that sputter obtains.
As shown in Figure 2, be the preceding current-time curvel that activates circulation for 55 times of present embodiment: activate in the circulation at first, can see in-0.5V position a peak having occurred; Activate in the circulation at second, can see in-0.2V position also having showed a peak; These two peaks are along with coming to a point that the increase that activates cycle index continues then, and activate in the circulation at the 11st and to have found the 3rd peak at the 0.5V place; It should be noted that at the peak of-0.2V position faster than other two peaks growths; Activate circulation since the 16th, second peak become suitable greatly.These three peaks are respectively by following reaction equation representative:
Ir+2H
2O-2e
-→Ir(OH)
2+2H
+ (1)
Ir(OH)
2+H
2O-e
-→Ir(OH)
3+H
+ (2)
Ir(OH)
3-e
-→IrO(OH)
2+H
+ (3)
That is to say, activate in the circulation at first that iridium is activated by galvanochemistry and is Ir (II) in-0.5V position; Activate in the circulation at second, more iridium is activated as Ir (II), and a part of Ir (II) is activated by galvanochemistry and is Ir (III) in-0.2V position; When the quantity of Ir (III) was abundant, the 3rd peak at 0.5V place occurred, and namely Ir (III) is activated as Ir (IV).
Activate in the circulation for 30 times in beginning, these three peaks become sharply simultaneously, and this is that the quantity of Ir (III) and Ir (IV) also is not enough to complete coated electrode point, so these three reactions can be carried out simultaneously because of the Ir (II) that is activated; Second peak activates circulation since the 16th and becomes suitable big, and this is because Ir (II) quantity that activates is enough, and reaction (2) can complete reaction; When activating circulation and reach 55 times, latter two peak comes to a point significantly and first peak becomes comparatively smooth, and this is because the Ir (II) that activates has covered the electrode points surface, has stoped iridium to be activated as Ir (II).Because the Ir (III) that activates is not enough to coated electrode point surface, reaction (2) is not affected with (3); First peak begins again to occur then, and this is because reaction (2) reacts away excessive Ir (II), and Ir (II) is not enough to covering surfaces, so reaction (1) begins again to take place.Therefore, three reactions can be carried out again simultaneously.
As shown in Figure 3, activate the current-time curvel of circulation for the 55-100 time for present embodiment: activate circulation up to the 105th time, the peak of-0.5V position is consistent being held also, illustrate that excessive problem does not take place Ir (II) again, consider Ir (II)/Ir (III), Ir (the III)/good oxidation peak of Ir (IV) has illustrated that reaction (2) and (3) have obtained acceleration.
As shown in Figure 4, be that present embodiment activates the current-time curvel of circulation for the 100-500 time: activate circulation time to the 145th time, a new peak occurred at-0.8V place, as reacting shown in (4); Simultaneously ,-0.2V position becomes more close with peak amplitude and the sharpness of-0.5V position, illustrates that the electrochemical activity of reaction (2) and (3) also becomes comparatively approaching.
2IrO
3+2H
2O-4e
-→2IrO(OH)
2+O
2 (4)
IrO(OH)
2-e
-→IrO
2(OH)+H
+ (5)
IrO
2(OH)-e
-→IrO
3+H
+ (6)
Reaction (5) occurs in 0.5V in the interval of 1V with (6), because the electrochemical activity of reaction (3) becomes higher, so more Ir (IV) is activated, further promoted carry out of reaction (5) with (6), because the peak of reaction (3) is very high, reaction (5) is slower with the speed of (6), so reaction (5) can be ignored with the peak of (6).
Along with the increase that activates cycle index, the peak of reaction (1) diminishes invisible up at 500 times the time gradually.The product that this explanation is activated has delayed the carrying out of reaction (1), until stopping, not having more iridium to be activated into high valence state; The peak of reaction (2) also broadens, and has become quite little in the time of 500 times.Reaction (2) is because the inhibition of reaction (1) also has been subjected to inhibition, and the peak of reaction (3) becomes quite sharp-pointed, and keeps stable.
As shown in Figure 5, be the variation of valence process of iridium in the present embodiment activation: when reaction (4) can be mentioned in the same breath with the peak of (3), reaction (3-6) had constituted circulation.Under this state, the activation of iridium is finished, and the yttrium oxide that is activated tends towards stability.
As shown in Figure 6, the SEM photo of the yttrium oxide film that activates for present embodiment iridium film, galvanochemistry: Fig. 6 (a) is the iridium film of sputter, shows smooth surface; And the yttrium oxide of Fig. 6 (b) for activating shows porous structure; Fig. 6 (c) is the enlarged drawing of Fig. 6 (b), demonstrates loose porous structure.This structure allows the quick exchange of hydrone and ion, is conducive to obtain higher charge storage.
As shown in Figure 7, for present embodiment activates the CV curve that circulates preceding 100 times: the iridium electrode that in-situ preparing obtains shows good fake capacitance character, after 10 activation circulations, begins to show wideer redox peak; Along with the increase that activates cycle index, the redox peak also becomes sharp-pointed more as reacts shown in (7), and the peak of negative sense is oxidation peak, and the peak of forward is reduction peak.
Activate in the circulation for 50 times in beginning, the CV curve has violent variation, shows that iridium is yttrium oxide by activation fast.From the 50-100 time activation circulation, the profile of CV curve remains unchanged, and has only the redox peak to continue to become big.
As shown in Figure 8, be present embodiment microelectrode charge storage and the preceding control graph of a relation that activates circulation for 100 times: the charge storage of the yttrium oxide microelectrode that is activated by galvanochemistry activates the relation of obeying y=0.08615x+1.9873 in the circulation with cycle index, r 100 times of beginning
2Be 0.9953.
As shown in Figure 9, activate the CV curve of circulation for the 100-500 time for present embodiment: from the 100-500 time activation circulation, the profile of CV curve remains unchanged substantially, has only the redox peak to continue to become big; Except the redox peak, it is big that other zones slowly become; After surpassing 500 activation circulations, the CV curve remains unchanged.
As shown in figure 10, activate the control graph of a relation of circulation for present embodiment microelectrode charge storage and the 100-500 time: the charge storage of the yttrium oxide microelectrode that is activated by galvanochemistry activates the relation of obeying y=0.07792x+3.082 in the circulation with cycle index, r at the 100th time to the 200th time
2Be 0.9924; The charge storage of the yttrium oxide microelectrode that is activated by galvanochemistry activates the relation of obeying y=0.07439x+3.298 in the circulation with cycle index, r at the 200th time to the 500th time
2Be 0.9935.
The preceding slope maximum that activates circulation for 100 times, the slope that activates circulation for the 100th time to the 200th time are that the preceding 100 times slope that activates circulation for 90%, the 200 time to the 500th time is preceding 100 times 86%.This quantitative result is consistent with the growth tendency in the activation.The charge storage of the yttrium oxide that activation is finished is 40.07mC/cm
2, being almost 24 times before activating, iridium electrode is 1.69mC/cm
2
As shown in figure 11, be present embodiment redox peak separation and the control graph of a relation that activates cycle index: in pH is 7 physiological saline, because the variation of oxide local pH causes the spacing at redox peak also to change; The spacing at definition redox peak is Δ Ep, and the variation of pH is that namely the activity of oxidation-reduction quality is more high owing to the release of proton in the reaction (3), consumption cause, and the variation of pH is more big; The redox peak separation of the yttrium oxide microelectrode that is activated by galvanochemistry with activate cycle index and obey following relation:
y=0.6541+0.00189x-8.875×10
-6x
2+2.1126×10
-8x
3-1.827×10
-11x
4
When the activation cycle index reaches 400 times, Δ E
pVariation become very little, this is that activation approaches another sign finish; Consider that charge storage is also increasing in the time of 500 times, this is because the iridium of high valence state is decomposed into steady I r (III)/Ir (IV), the activity of oxidation-reduction quality changes maximum in preceding 100 times are activated, change in second 100 activation and take second place, activate the variation minimum last 300 times, this variation tendency with charge storage is consistent.
As shown in figure 12, activate the impedance magnitude curve that circulates preceding 100 times for present embodiment: in 10 activation of beginning, violent variation takes place in impedance magnitude; Activate in the circulation at 10-100 time, keep stable above impedance magnitude behind the 10kHz.And showing capacitive properties in low-frequency range, this can draw from the slope of curve approaching-1; In 30 activation of beginning, the speed that impedance magnitude changes is very fast, and in this stage, iridium is activated fast, and the oxide of iridium grows out of nothing.So this stage is bigger to the influence of impedance magnitude; Up to the 100th activation circulation, the speed that impedance magnitude changes is more and more slower, and this is because with respect to the incipient stage, the iridium of each activation cyclic activation tends towards stability in the follow-up activation.
As shown in figure 13, activate the impedance magnitude curve of circulation for the 100-500 time for present embodiment: activate in the circulation at 100-250 time, keep relative stability above impedance magnitude behind the 1kHz; Activate in the circulation at 250-500 time, the lower limit in the zone that keeps relative stability drops to 100Hz; Show the character of electric capacity equally in low-frequency range; But the variation of impedance magnitude is very little, and this explanation the approaching of activation is finished, so impedance magnitude also is a factor can controlling in the activation.
As shown in figure 14, be present embodiment 1kHz impedance magnitude and the control graph of a relation that activates cycle index: the 1kHz impedance magnitude of the yttrium oxide microelectrode that is activated by galvanochemistry with activate cycle index and obey y=-3291 * 0.9790
x+ 4321 relation, after activation was finished, impedance magnitude was near 4300 ohm.
As shown in figure 15, be present embodiment electric double layer capacitance and the control graph of a relation that activates cycle index: be the impedance magnitude at 1 place according to angular frequency, the approximate treatment electric double layer capacitance, the electric double layer capacitance of the yttrium oxide microelectrode that is activated by galvanochemistry with activate cycle index and obey y=2.962 * 10
-9X+6.531 * 10
-8Relation, r
2Be 0.9940.Take all factors into consideration the variation tendency of charge storage, electric double layer capacitance can be used as an index of electrochemical activity in the activation.
As shown in figure 16, activate the impedance angle curve that circulates preceding 100 times for present embodiment: before the un-activation, iridium electrode shows typical fake capacitance character; After ten activation, begin to embody electrical resistance property at high band, activate in the circulation at 10-50 time, the starting point in resistive zone moves to left continuously, activates in the circulation at 50-100 time, and high band shows stronger electrical resistance property.
As shown in figure 17, activate the impedance angle curve of circulation for the 100-500 time for present embodiment: activate in the circulation at 100-250 time, resistive zone enlarges continuously, and shows stronger capacitive properties in low-frequency range; At last, activating in the circulation at 25-500 time, tends towards stability in resistive zone and capacitive zone, and activation is finished gradually.
As shown in figure 18, be present embodiment 1kHz impedance angle and the control graph of a relation that activates cycle index: the 1kHz impedance angle of the yttrium oxide microelectrode that is activated by galvanochemistry with activate cycle index and obey y=-8.609-59.57 * 0.9611
xRelation, activate finish after, the 1kHz impedance angle approaches-8.6 degree.
As shown in figure 19, be present embodiment capacitive maximum point and resistive maximum point and the control graph of a relation that activates cycle index: the capacitive maximum point of the yttrium oxide microelectrode that is activated by galvanochemistry with activate cycle index and obey y=-87.10+11.24 * 0.9487
xRelation, activate finish after, capacitive maximum point phase angle approaches-87.10 degree; The resistive maximum point of the yttrium oxide microelectrode that is activated by galvanochemistry with activate cycle index and obey y=-6.629-16.22 * 0.9842
xRelation, activate finish after, resistive maximum point phase angle approaches-6.629 degree.Therefore have more this quantitative relationship, capacitive maximum point and resistive maximum point also are subjected to activating the control of cycle index in activation.
In sum, utilize the preparation method of the yttrium oxide microelectrode that is activated by galvanochemistry, can be according to the electrochemical properties of the strict control of the quantitative relationship that obtains microelectrode.Activate or activate again for original position, can use minimum activation number of times to realize the electrochemical properties that needs, reduce and activate the additional injury that produces.
More than specific embodiments of the invention are described.It will be appreciated that the present invention is not limited to above-mentioned specific implementations, those skilled in the art can make various distortion or modification within the scope of the claims, and this does not influence flesh and blood of the present invention.
Claims (9)
1. preparation method by the yttrium oxide microelectrode that activates the cycle control electrochemical properties, it is characterized in that, the iridium microelectrode array galvanochemistry that described method utilizes sputter to obtain activates and is yttrium oxide, working electrolyte is physiological saline, Activiation method is working electrode voltage at-1V to+1V scanning, sweep velocity is 100mV/s, and run-down is a cycle index.
2. the preparation method of yttrium oxide microelectrode according to claim 1 is characterized in that, the concrete preparation process of described iridium microelectrode array is as follows:
At first get rid of the positive glue of 5 μ m and graphical at the Si sheet, the sputtered titanium Seed Layer, the 100-1000 dust, splash-proofing sputtering metal iridium 300 nanometers adopt Lift-off technology to remove photoresist again, graphical Seed Layer and iridium metals layer formation electrode;
And then the polychlorostyrene that deposits 5 μ m is for the second time graphical photoresist for the P-xylene film, uses reactive ion etching that polychlorostyrene is carved for the P-xylene film and wears, and exposes electrode points, constitutes the microelectrode array overlayer; So just prepared the iridium microelectrode array;
Before next step carried out galvanochemistry activation yttrium oxide microelectrode array, the iridium microelectrode array must pass through 10 minutes the ultrasonic cleaning respectively of acetone, alcohol, deionized water.
3. the preparation method of yttrium oxide microelectrode according to claim 1 and 2, it is characterized in that, the working electrolyte that described galvanochemistry activates is physiological saline, Activiation method is working electrode voltage at-1V to+1V scanning, sweep velocity is 100mV/s, run-down is a cycle index, and namely 20 seconds is the time of a circulation; Contrast electrode is the Ag/AgCl electrode, is the platinized platinum electrode to electrode.
4. the preparation method of yttrium oxide microelectrode according to claim 3 is characterized in that, the scope of charge storage before and after galvanochemistry activates of the described yttrium oxide microelectrode that is activated by galvanochemistry is 1.69-40.07mC/cm
2
5. the preparation method of yttrium oxide microelectrode according to claim 4, it is characterized in that, the charge storage of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=0.08615x+1.9873 in the control method that 100 times of beginning activate in the circulation, x is cycle index, and y is charge storage;
The charge storage of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=0.07792x+3.082 in the control method that activates in the circulation for the 100th time to the 200th time, and x is cycle index, and y is charge storage;
The charge storage of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=0.07439x+3.298 in the control method that activates in the circulation for the 200th time to the 500th time, and x is cycle index, and y is charge storage.
6. the preparation method of yttrium oxide microelectrode according to claim 4 is characterized in that, the control method of the redox peak separation of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=0.6541+0.00189x-8.875 * 10
-6x
2+ 2.1126 * 10
-8x
3-1.827 * 10
-11x
4, x is cycle index, y is the redox peak separation;
The control method of the 1kHz impedance magnitude of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=-3291 * 0.9790
x+ 4321, x is cycle index, and y is the 1kHz impedance magnitude;
The control method of the 1kHz impedance angle of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=-8.609-59.57 * 0.9611
x, x is cycle index, y is the 1kHz impedance angle.
7. according to the preparation method of each described yttrium oxide microelectrode of claim 4-6, it is characterized in that the control method of the electric double layer capacitance of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=2.962 * 10
-9X+6.531 * 10
-8, x is cycle index, y is electric double layer capacitance.
8. according to the preparation method of each described yttrium oxide microelectrode of claim 4-6, it is characterized in that the control method of the capacitive maximum point of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=-87.10+11.24 * 0.9487
x, x is cycle index, y is the capacitive maximum point.
9. according to the preparation method of each described yttrium oxide microelectrode of claim 4-6, it is characterized in that the control method of the resistive maximum point of the described yttrium oxide microelectrode that is activated by galvanochemistry is y=-6.629-16.22 * 0.9842
x, x is cycle index, y is resistive maximum point.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310190510.5A CN103293204B (en) | 2013-05-21 | 2013-05-21 | Preparation method of iridium oxide microelectrode controlling electrochemical property by using activated circulation |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20060148254A1 (en) * | 2005-01-05 | 2006-07-06 | Mclean George Y | Activated iridium oxide electrodes and methods for their fabrication |
| CN101057780A (en) * | 2007-05-18 | 2007-10-24 | 武汉大学 | Iridium oxide electrode and its manufacturing method |
| CN102495117A (en) * | 2011-12-19 | 2012-06-13 | 天津理工大学 | Method for improving repeatability of working electrode and application of method |
| CN102788828A (en) * | 2012-07-19 | 2012-11-21 | 北京科技大学 | IrOx electrode prepared through cyclic thermo oxidation method |
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Patent Citations (4)
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|---|---|---|---|---|
| US20060148254A1 (en) * | 2005-01-05 | 2006-07-06 | Mclean George Y | Activated iridium oxide electrodes and methods for their fabrication |
| CN101057780A (en) * | 2007-05-18 | 2007-10-24 | 武汉大学 | Iridium oxide electrode and its manufacturing method |
| CN102495117A (en) * | 2011-12-19 | 2012-06-13 | 天津理工大学 | Method for improving repeatability of working electrode and application of method |
| CN102788828A (en) * | 2012-07-19 | 2012-11-21 | 北京科技大学 | IrOx electrode prepared through cyclic thermo oxidation method |
Non-Patent Citations (1)
| Title |
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| DAVID J. COMSTOCK ET. AL: "Synthesis of nanoporous activated oxide films by anodized aluminum oxide templated atomic layer deposition", 《ELECTROCHEMISTRY COMMUNICATIONS》, no. 12, 31 August 2010 (2010-08-31), pages 1543 - 1546 * |
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