CN103293204B - 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
- Publication number
- CN103293204B CN103293204B CN201310190510.5A CN201310190510A CN103293204B CN 103293204 B CN103293204 B CN 103293204B CN 201310190510 A CN201310190510 A CN 201310190510A CN 103293204 B CN103293204 B CN 103293204B
- Authority
- CN
- China
- Prior art keywords
- yttrium oxide
- microelectrode
- activated
- galvanochemistry
- cycle index
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Semiconductor Memories (AREA)
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 of activation cycle control electrochemical properties.
Background technology
In recent years, along with the continuous progress of MEMS (micro electro mechanical system) (MEMS:Micro-Electro-Mechanical Systems) technology, the micro-system such as microelectronic device and microsensor range of application is constantly expanded, has been widely used in multiple field, particularly medical domain.
The microelectrode prepared by materials such as noble metal platinum, gold and iridium utilizes micro electro mechanical system (MEMS) technology at a typical apply of biomedical aspect.Based on iridium, obtained the method for yttrium oxide by electrochemical method, equipment, the method for needs are simple, obtain the attention of Many researchers.But the strict quantitative relationship of the character of the yttrium oxide activated by electrochemical method and Activiation method, then do not receive attention.
China's application number 200710052206.9, application publication number CN 101057780, 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 pH sensor.Iridium oxide electrode of the present invention has an insulation course, wherein at least encapsulates an electrode cores; Described electrode cores be one at least one end be have reactivation on metal iridium bottom to generate the electric conductor on yttrium oxide top layer at metal iridium or non-iridium metals outside deposition, its one end is connected with wire, and yttrium oxide top layer is exposed outside insulation course.This electrode is obtained by iridium metals silk, but all not providing galvanochemistry in this patent and prior art activates the control method with yttrium oxide character.So, in actual use, should use and be subject to more restriction.
To sum up, although the preparation method of the yttrium oxide microelectrode array that galvanochemistry activates obtains certain research, but have no the character of yttrium oxide and the control device of Activiation method of the activation of report electrochemical method in document, therefore, the invention provides a kind of preparation method of yttrium oxide microelectrode, solve this problem.
Summary of the invention
For defect of the prior art, the object of this invention is to provide a kind of preparation method of yttrium oxide microelectrode by activating cycle control electrochemical properties, easy and simple to handle, can the electrochemical properties of strict controlled oxidization iridium microelectrode array.And the character of the yttrium oxide that can be activated by electrochemical method and the control planning original position of Activiation method reactivate yttrium oxide.
For achieving the above object, the invention provides a kind of preparation method by the yttrium oxide microelectrode of activation cycle control electrochemical properties, described method utilizes and sputters the iridium microelectrode array galvanochemistry activation obtained is yttrium oxide, working electrolyte is physiological saline, Activiation method is that working electrode voltage is in-1V to+1V scanning, sweep velocity is 100mV/s (millivolt is per second), and run-down is a cycle index.
Preferably, the concrete preparation process of described iridium microelectrode array is as follows:
First the positive glue getting rid of 5 μm on Si sheet is also graphical, sputtered titanium Seed Layer, 100-1000 dust, then splash-proofing sputtering metal iridium 300 nanometer, and adopt Lift-off technique to remove photoresist, graphical Seed Layer and iridium metals layer form electrode;
And then depositing the Parylene-C of 5 μm, second time, photoetching offset plate figure, uses reactive ion etching (RIE) that Parylene-C is carved and wears, expose electrode points, form microelectrode array overlayer; So just prepare iridium microelectrode array;
Before next step carries out galvanochemistry activation yttrium oxide microelectrode array, iridium microelectrode array has to pass through acetone, alcohol, the ultrasonic cleaning of 10 minutes of deionized water difference.
Preferably, the concrete galvanochemistry Activiation method that described galvanochemistry activates yttrium oxide microelectrode array is as follows:
The working electrolyte that galvanochemistry activates is physiological saline, and Activiation method is that working electrode voltage scans at-1V to+1V, and sweep velocity is 100mV/s (millivolt is per second), and run-down is a cycle index, namely within 20 seconds, is the time of a circulation; Contrast electrode is Ag/AgCl electrode, is platinum plate electrode to electrode.
Preferably, the scope of charge storage before and after galvanochemistry activates of the described yttrium oxide microelectrode activated by galvanochemistry is 1.69-40.07mC/cm
2.
Preferably, the charge storage of the described yttrium oxide microelectrode activated by galvanochemistry the control method activated in circulation for 100 times be y=0.08615x+1.9873, x be cycle index, y is charge storage.
Preferably, the charge storage of the described yttrium oxide microelectrode activated by galvanochemistry is y=0.07792x+3.082, x in the control method that the 100th time to the 200th time is activated in circulation is cycle index, and y is charge storage.
Preferably, the charge storage of the described yttrium oxide microelectrode activated by galvanochemistry is y=0.07439x+3.298, x in the control method that the 200th time to the 500th time is activated in circulation is cycle index, and y is charge storage.
Preferably, the control method of the redox peak separation of the described yttrium oxide microelectrode activated by galvanochemistry is y1=0.6541+0.00189x-8.875 × 10
-6x
2+ 2.1126 × 10
-8x
3-1.827 × 10
-11x
4, x is cycle index, and y1 is redox peak separation.
Preferably, the control method of the 1kHz impedance magnitude of the described yttrium oxide microelectrode activated by galvanochemistry is y2=-3291 × 0.9790
x+ 4321, y2 is 1kHz impedance magnitude.
Preferably, the control method of the 1kHz impedance angle of the described yttrium oxide microelectrode activated by galvanochemistry is y3=-8.609-59.57 × 0.9611
x, y3 is 1kHz impedance angle.
Preferably, the control method of the electric double layer capacitance of the described yttrium oxide microelectrode activated by galvanochemistry is y4=2.962 × 10
-9x+6.531 × 10
-8, x is cycle index, and y4 is electric double layer capacitance.
Preferably, the control method of the capacitive maximum point of the described yttrium oxide microelectrode activated by galvanochemistry is y5=-87.10+11.24 × 0.9487
x, x is cycle index, and y5 is capacitive maximum point.
Preferably, the control method of the resistive maximum point of the described yttrium oxide microelectrode activated by galvanochemistry is y6=-6.629-16.22 × 0.9842
x, x is cycle index, and y6 is resistive maximum point.
Compared with prior art, the present invention has following beneficial effect:
Preparation method of the present invention be utilize micro-processing technology to prepare iridium microelectrode array, electrochemical method activate the character of yttrium oxide and the strict quantitative relationship of Activiation method.The present invention is easy and simple to handle, can the electrochemical properties of strict controlled oxidization iridium microelectrode array; The electrochemical properties of microelectrode strictly can be controlled according to the quantitative relationship obtained; Original position is activated or reactivation, minimum activation number of times can be used to realize the electrochemical properties needed, reduce the additional injury activating and produce.
Accompanying drawing explanation
By reading the detailed description done non-limiting example with reference to the following drawings, other features, objects and advantages of the present invention will become more obvious:
Fig. 1 is the SEM photo of one embodiment of the invention iridium microelectrode electrode points;
Fig. 2 is the front current-time curvel activating circulation for 55 times of one embodiment of the invention;
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;
The SEM photo of the yttrium oxide film that Fig. 6 is one embodiment of the invention iridium film, galvanochemistry activates;
Fig. 7 is the front CV curve activating circulation for 100 times of one embodiment of the invention;
Fig. 8 is one embodiment of the invention microelectrode charge storage and activates the graph of a relation circulated first 100 times;
Fig. 9 is the CV curve that one embodiment of the invention activates circulation for the 100-500 time;
Figure 10 is one embodiment of the invention microelectrode charge storage and activates the graph of a relation circulated the 100-500 time;
Figure 11 is one embodiment of the invention redox peak separation and the graph of a relation activating cycle index;
Figure 12 is the front impedance magnitude curve activating circulation for 100 times of one embodiment of the invention;
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 activating cycle index;
Figure 15 is one embodiment of the invention electric double layer capacitance and the graph of a relation activating cycle index;
Figure 16 is the front impedance angle curve activating circulation for 100 times of one embodiment of the invention;
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 activating cycle index;
Figure 19 is the graph of a relation of one embodiment of the invention capacitive maximum point and resistive maximum point and activation cycle index.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
Embodiment 1
The preparation method of the described yttrium oxide microelectrode activated by galvanochemistry be utilize micro-processing technology to prepare iridium microelectrode array, electrochemical method activate the character of yttrium oxide and the strict quantitative relationship of Activiation method, described strict quantitative relationship is in physiological saline, working electrode voltage obtains in-1V to+1V scanning, and run-down is a cycle index.
The concrete preparation process of described iridium microelectrode array is as follows:
First the positive glue getting rid of 5 μm on Si sheet is also graphical, sputtered titanium Seed Layer, 100-1000 dust, then splash-proofing sputtering metal iridium 300 nanometer, and adopt Lift-off technique to remove photoresist, graphical Seed Layer and iridium metals layer form electrode;
And then depositing the Parylene-C of 5 μm, second time, photoetching offset plate figure, uses reactive ion etching (RIE) that Parylene-C is carved and wears, expose electrode points, form microelectrode array overlayer; So just prepare iridium microelectrode array;
Before next step carries out galvanochemistry activation yttrium oxide microelectrode array, iridium microelectrode array has to pass through acetone, alcohol, the ultrasonic cleaning of 10 minutes of deionized water difference.
The concrete galvanochemistry Activiation method that described galvanochemistry activates yttrium oxide microelectrode array is as follows:
The working electrolyte that galvanochemistry activates is physiological saline, and Activiation method is that working electrode voltage scans at-1V to+1V, and sweep velocity is 100mV/s (millivolt is per second), and run-down is a cycle index, namely within 20 seconds, is the time of a circulation; Contrast electrode is Ag/AgCl electrode, is large-area platinum plate electrode to electrode.
Embodiment 2
As shown in Figure 1, the SEM photo for the present embodiment iridium microelectrode electrode points: the diameter of electrode points is 100 microns, this is in the typical electrode points application size of electro physiology application one, and the iridium of the present embodiment is that sputtering obtains.
As shown in Figure 2, be the front current-time curvel activating circulation for 55 times of the present embodiment: activate in circulation at first, can see and occur a peak in-0.5V position; Activate in circulation at second, can see and also show a peak in-0.2V position; What then these two peaks continued along with the increase activating cycle index comes to a point, and has found the 3rd peak at 0.5V place in the 11st activation circulation; It should be noted that faster than other two peaks growths of peak in-0.2V position; Activating circulation from the 16th, second peak becomes suitable large.These three peaks are represented by following reaction equation respectively:
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, activate in circulation at first, iridium is activated as Ir (II) in-0.5V position by galvanochemistry; Activate in circulation at second, more iridium is activated as Ir (II), and a part of Ir (II) is activated as Ir (III) in-0.2V position by galvanochemistry; Until when the quantity of Ir (III) is abundant, the 3rd peak at 0.5V place occurs, namely Ir (III) is activated as Ir (IV).
Activate in circulation at 30 times that start, these three peaks become sharp-pointed simultaneously, this is because the quantity of the Ir be activated (II), Ir (III) and Ir (IV) is also not enough to complete coated electrode point, so these three reactions can be carried out simultaneously; Second peak becomes suitable large activating circulation from the 16th, this is because Ir (II) quantity activated is enough, reaction (2) can complete reaction; When activating circulation and reaching 55 times, latter two peak comes to a point significantly and first peak becomes comparatively smooth, this is because the Ir (II) activated covers electrode points surface, prevents iridium to be activated as Ir (II).Because the Ir (III) activated is not enough to coated electrode point surface, reaction (2) and (3) are not affected; Then first peak starts again to occur, this is that Ir (II) is not enough to covering surfaces because reaction (2) reacts away excessive Ir (II), so reaction (1) starts again to occur.Therefore, three reactions can be carried out again simultaneously.
As shown in Figure 3, for the present embodiment activates the current-time curvel of circulation for the 55-100 time: until the 105th time is activated circulation, the peak of-0.5V position is also unanimously kept, illustrate that Ir (II) excessive problem does not occur again, consider Ir (II)/Ir (III), the oxidation peak that Ir (III)/Ir (IV) is good, describes reaction (2) and obtains acceleration with (3).
As shown in Figure 4, for the present embodiment activates the current-time curvel of circulation for the 100-500 time: activate circulation time to the 145th time, occurred a new peak at-0.8V place, as shown in reaction (4); Meanwhile ,-0.2V position becomes more close with the peak amplitude of-0.5V position with sharpness, illustrates that reaction (2) also becomes comparatively close with the electrochemical activity of (3).
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) and (6) occur in the interval of 0.5V to 1V, because the electrochemical activity reacting (3) becomes higher, so more Ir (IV) is activated, further promote the carrying out of reaction (5) and (6), because the peak reacting (3) is very high, reaction (5) is comparatively slow with the speed of (6), so reaction (5) can be ignored with the peak of (6).
Along with the increase activating cycle index, the peak of reaction (1) diminishes gradually until invisible 500 times time.This illustrates that the product be activated has delayed the carrying out of reaction (1), until stop, not having more iridium to be activated into high-valence state; Reaction (2) peak also broaden, until 500 times time become quite little.Reaction (2) also receives suppression due to the suppression of reacting (1), and the peak reacting (3) becomes quite sharp-pointed, and keeps stable.
As shown in Figure 5, the variation of valence process for iridium in the present embodiment activation: when reacting (4) peak with (3) and can mentioning in the same breath, reaction (3-6) constitutes circulation.Under this state, the activation of iridium completes, and the yttrium oxide be activated tends towards stability.
As shown in Figure 6, be the SEM photo of the yttrium oxide film of the present embodiment iridium film, galvanochemistry activation: Fig. 6 (a) is the iridium film of sputtering, shows smooth surface; And Fig. 6 (b) is the yttrium oxide activated, show porous structure; The enlarged drawing that Fig. 6 (c) is Fig. 6 (b), demonstrates loose porous structure.This structure allows the quick exchange of hydrone and ion, is conducive to obtaining higher charge storage.
As shown in Figure 7, the CV curve activating circulation for 100 times for the present embodiment is front: the iridium electrode that original position prepares shows good fake capacitance character, after activating circulation 10 times, starts to show wider redox peak; Along with the increase activating cycle index, redox peak also becomes more sharp-pointed as shown in reaction (7), and the peak of negative sense is oxidation peak, and the peak of forward is reduction peak.
Activate in circulation at 50 times that start, CV curve has violent change, and display iridium is activated fast as yttrium oxide.Activate circulation from the 50-100 time, the profile of CV curve remains unchanged, and only has redox peak to continue to become large.
As shown in Figure 8, for the present embodiment microelectrode charge storage and frontly activate the control planning figure circulated for 100 times: the charge storage of the yttrium oxide microelectrode activated by galvanochemistry activate for 100 times circulate in obey the relation of y=0.08615x+1.9873, r with cycle index
2be 0.9953.
As shown in Figure 9, for the present embodiment activates the CV curve of circulation for the 100-500 time: activate circulation from the 100-500 time, the profile of CV curve remains unchanged substantially, redox peak is only had to continue to become large; Except redox peak, other regions slowly become large; After activating circulation more than 500 times, CV curve remains unchanged.
As shown in Figure 10, for the present embodiment microelectrode charge storage and activate the control planning figure circulated for the 100-500 time: the charge storage of the yttrium oxide microelectrode activated by galvanochemistry to activate for the 100th time to the 200th time circulate in obey the relation of y=0.07792x+3.082, r with cycle index
2be 0.9924; The charge storage of the yttrium oxide microelectrode activated by galvanochemistry activates the relation of obeying y=0.07439x+3.298 in circulation with cycle index at the 200th time to the 500th time, r
2be 0.9935.
The front slope activating circulation for 100 times is maximum, the slope activating circulation for the 100th time to the 200th time to be the slope first 100 times the 90%, 200th time to the 500th time activating circulation be first 100 times 86%.This quantitative result is consistent with the growth tendency in activation.The charge storage of the yttrium oxide activated is 40.07mC/cm
2, be almost 24 times before activation, iridium electrode is 1.69mC/cm
2.
As shown in figure 11, be the present embodiment redox peak separation and the control planning figure activating cycle index: be in the physiological saline of 7 at pH, the change due to oxide local pH causes the spacing at redox peak also to change; The spacing at definition redox peak is Δ E
p, the change of pH be due to proton in reaction (3) release, consume and cause, namely the activity of oxidation-reduction quality is higher, and the change of pH is larger; The redox peak separation of the yttrium oxide microelectrode activated by galvanochemistry obeys following relation with activation cycle index:
y1＝0.6541+0.00189x-8.875×10
-6x
2+2.1126×10
-8x
3-1.827×10
-11x
4
When activating cycle index and reaching 400 times, Δ E
pchange become very little, this is activation close to another mark completed; Consider charge storage up to 500 times time also in increase, this is because the iridium of high-valence state is decomposed into stable Ir (III)/Ir (IV), the activity of oxidation-reduction quality changes maximum in front 100 activation, change in second 100 activation and take second place, last 300 activation changes are minimum, and this is consistent with the variation tendency of charge storage.
As shown in figure 12, the impedance magnitude curve activating circulation for 100 times for the present embodiment is front: in activating at 10 times that start, violent change occurs impedance magnitude; Activate in circulation at 10-100 time, keep stable more than impedance magnitude after 10kHz.And showing capacitive properties in low-frequency range, this can draw from the slope of curve close-1; In activating at 30 times that start, the speed of impedance magnitude change, in this stage, iridium is activated fast, and the oxide of iridium grows out of nothing.So the impact of this stage on impedance magnitude is larger; Until the 100th time is activated circulation, the speed goes of impedance magnitude change is slow, and this is due to relative to the incipient stage, and in subsequent activation, the iridium of each activation cyclic activation tends towards stability.
As shown in figure 13, for the present embodiment activates the impedance magnitude curve of circulation for the 100-500 time: activate in circulation at 100-250 time, keep relative stability more than impedance magnitude after 1kHz; Activate in circulation at 250-500 time, the lower limit in the region that keeps relative stability drops to 100Hz; The character of electric capacity is shown equally in low-frequency range; But the change of impedance magnitude is very little, this illustrates that the close of activation completes, so impedance magnitude is also a factor that can control in activation.
As shown in figure 14, be the present embodiment 1kHz impedance magnitude and the control planning figure activating cycle index: the 1kHz impedance magnitude of the yttrium oxide microelectrode activated by galvanochemistry obeys y2=-3291 × 0.9790 with activation cycle index
xthe relation of+4321, after having activated, impedance magnitude is close to 4300 ohm.
As shown in figure 15, for the present embodiment electric double layer capacitance with activate the control planning figure of cycle index: the impedance magnitude according to angular frequency being 1 place, approximate treatment electric double layer capacitance, the electric double layer capacitance of the yttrium oxide microelectrode activated by galvanochemistry obeys y4=2.962 × 10 with activation cycle index
-9x+6.531 × 10
-8relation, r
2be 0.9940.Consider the variation tendency of charge storage, electric double layer capacitance can as of electrochemical activity in an activation index.
As shown in figure 16, the impedance angle curve activating circulation for 100 times for the present embodiment is front: before un-activation, iridium electrode shows typical fake capacitance character; After ten times are activated, start to embody electrical resistance property at high band, activate in circulation at 10-50 time, the starting point of resistive region moves to left continuously, and activate in circulation at 50-100 time, high band shows stronger electrical resistance property.
As shown in figure 17, for the present embodiment activates the impedance angle curve of circulation for the 100-500 time: activate in circulation at 100-250 time, resistive region expands continuously, and shows stronger capacitive properties in low-frequency range; Finally, activate in circulation at 25-500 time, tend towards stability in resistive region and capacitive region, activation completes gradually.
As shown in figure 18, be the present embodiment 1kHz impedance angle and the control planning figure activating cycle index: the 1kHz impedance angle of the yttrium oxide microelectrode activated by galvanochemistry obeys y3=-8.609-59.57 × 0.9611 with activation cycle index
xrelation, after having activated, 1kHz impedance angle close-8.6 degree.
As shown in figure 19, be the present embodiment capacitive maximum point and resistive maximum point and the control planning figure activating cycle index: the capacitive maximum point of the yttrium oxide microelectrode activated by galvanochemistry with activate cycle index and obey y5=-87.10+11.24 × 0.9487
xrelation, after having activated, capacitive maximum point phase angle close-87.10 degree; The resistive maximum point of the yttrium oxide microelectrode activated by galvanochemistry obeys y6=-6.629-16.22 × 0.9842 with activation cycle index
xrelation, after having activated, resistive maximum point phase angle close-6.629 degree.Therefore have more this quantitative relationship, capacitive maximum point and resistive maximum point are also subject to the control activating cycle index in activation.
In sum, utilize the preparation method of the yttrium oxide microelectrode activated by galvanochemistry, strictly can control the electrochemical properties of microelectrode according to the quantitative relationship obtained.Original position is activated or reactivation, minimum activation number of times can be used to realize the electrochemical properties needed, reduce the additional injury activating and produce.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (8)
1. one kind by the preparation method of yttrium oxide microelectrode activating cycle control electrochemical properties, it is characterized in that, described method utilizes and sputters the iridium microelectrode array galvanochemistry activation obtained is yttrium oxide, working electrolyte is physiological saline, Activiation method is that working electrode voltage is in-1V to+1V scanning, sweep velocity is 100mV/s, and run-down is a cycle index;
The concrete preparation process of described iridium microelectrode array is as follows:
First the positive glue getting rid of 5 μm on Si sheet is also graphical, sputtered titanium Seed Layer, 100-1000 dust, then splash-proofing sputtering metal iridium 300 nanometer, and adopt Lift-off technique to remove photoresist, graphical Seed Layer and iridium metals layer form electrode;
And then depositing the Parylene C film of 5 μm, second time, photoetching offset plate figure, uses reactive ion etching that Parylene C film is carved and wears, expose electrode points, form microelectrode array overlayer; So just prepare iridium microelectrode array;
Before next step carries out galvanochemistry activation yttrium oxide microelectrode array, iridium microelectrode array has to pass through acetone, alcohol, the ultrasonic cleaning of 10 minutes of deionized water difference.
2. the preparation method of yttrium oxide microelectrode according to claim 1, it is characterized in that, the working electrolyte that described galvanochemistry activates is physiological saline, Activiation method is that working electrode voltage is in-1V to+1V scanning, sweep velocity is 100mV/s, run-down is a cycle index, namely within 20 seconds, is the time of a circulation; Contrast electrode is Ag/AgCl electrode, is platinum plate electrode to electrode.
3. the preparation method of yttrium oxide microelectrode according to claim 2, is characterized in that, the scope of charge storage before and after galvanochemistry activates of the described yttrium oxide microelectrode activated by galvanochemistry is 1.69-40.07mC/cm
2.
4. the preparation method of yttrium oxide microelectrode according to claim 3, it is characterized in that, the charge storage of the described yttrium oxide microelectrode activated by galvanochemistry the control method activated in circulation for 100 times be y=0.08615x+1.9873, x is cycle index, and y is charge storage;
The charge storage of the described yttrium oxide microelectrode activated by galvanochemistry is y=0.07792x+3.082, x in the control method that the 100th time to the 200th time is activated in circulation is cycle index, and y is charge storage;
The charge storage of the described yttrium oxide microelectrode activated by galvanochemistry is y=0.07439x+3.298, x in the control method that the 200th time to the 500th time is activated in circulation is cycle index, and y is charge storage.
5. the preparation method of yttrium oxide microelectrode according to claim 3, is characterized in that, the control method of the redox peak separation of the described yttrium oxide microelectrode activated by galvanochemistry is y1=0.6541+0.00189x-8.875 × 10
-6x
2+ 2.1126 × 10
-8x
3-1.827 × 10
-11x
4, x is cycle index, and y1 is redox peak separation;
The control method of the 1kHz impedance magnitude of the described yttrium oxide microelectrode activated by galvanochemistry is y2=-3291 × 0.9790
x+ 4321, x is cycle index, and y2 is 1kHz impedance magnitude;
The control method of the 1kHz impedance angle of the described yttrium oxide microelectrode activated by galvanochemistry is y3=-8.609-59.57 × 0.9611
x, x is cycle index, and y3 is 1kHz impedance angle.
6. the preparation method of the yttrium oxide microelectrode according to any one of claim 3-5, is characterized in that, the control method of the electric double layer capacitance of the described yttrium oxide microelectrode activated by galvanochemistry is y4=2.962 × 10
-9x+6.531 × 10
-8, x is cycle index, and y4 is electric double layer capacitance.
7. the preparation method of the yttrium oxide microelectrode according to any one of claim 3-5, is characterized in that, the control method of the capacitive maximum point of the described yttrium oxide microelectrode activated by galvanochemistry is y5=-87.10+11.24 × 0.9487
x, x is cycle index, and y5 is capacitive maximum point.
8. the preparation method of the yttrium oxide microelectrode according to any one of claim 3-5, is characterized in that, the control method of the resistive maximum point of the described yttrium oxide microelectrode activated by galvanochemistry is y6=-6.629-16.22 × 0.9842
x, x is cycle index, and y6 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 |
Applications Claiming Priority (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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103293204A CN103293204A (en) | 2013-09-11 |
| CN103293204B true CN103293204B (en) | 2015-01-21 |
Family
ID=49094440
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310190510.5A Active CN103293204B (en) | 2013-05-21 | 2013-05-21 | Preparation method of iridium oxide microelectrode controlling electrochemical property by using activated circulation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103293204B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2013
- 2013-05-21 CN CN201310190510.5A patent/CN103293204B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|
| Synthesis of nanoporous activated oxide films by anodized aluminum oxide templated atomic layer deposition;David J. Comstock et. al;《Electrochemistry Communications》;20100831(第12期);1543-1546 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103293204A (en) | 2013-09-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106667475B (en) | A kind of implanted flexible nervus comb and preparation method thereof and method for implantation | |
| Lu et al. | Anodically electrodeposited iridium oxide films microelectrodes for neural microstimulation and recording | |
| Harris et al. | Conducting polymer coated neural recording electrodes | |
| Gong et al. | Materials-driven soft wearable bioelectronics for connected healthcare | |
| Harris et al. | Measuring the effective area and charge density of platinum electrodes for bionic devices | |
| CN105063400B (en) | It is a kind of to use the Ti/TiO with nano-porous structure2The method that composite prepares ultracapacitor | |
| Yoon et al. | Aligned nanowire growth using lithography-assisted bonding of a polycarbonate template for neural probe electrodes | |
| US20210370053A1 (en) | Neuro-stimulation and Sensor Devices Comprising Low-Impedance Electrodes, and Methods, Systems And Uses Thereof | |
| CN108125677B (en) | Microelectrode and preparation method thereof | |
| EP2674393B1 (en) | Device and method for micro-stimulation for and data acquisition from biological cells | |
| CN104465125B (en) | TiO2Three-dimensional interdigital microelectrodes of/NiO and preparation method thereof | |
| CN109350846A (en) | A kind of functionalization wide cut implantation micro-electrode array and the preparation method and application thereof | |
| Rui et al. | Parylene-based implantable Pt-black coated flexible 3-D hemispherical microelectrode arrays for improved neural interfaces | |
| US20190010627A1 (en) | Method for treating a surface of a metallic structure | |
| CN106037719B (en) | Platinum nanowire modified microelectrode array and preparation method thereof | |
| CN104777203A (en) | Preparation method of Pt-Ni alloy nano tube array electrode and application for enzyme-free glucose sensor | |
| CN110074758A (en) | Formula is tatooed without underlayer electrode preparation method and device based on multi-layer graphene | |
| EP2800589B1 (en) | Porous dealloyed electrodes | |
| CN106419906B (en) | Iridium oxide/platinum nano-column composite coating modified microelectrode array and preparation method thereof | |
| CN107638176A (en) | A kind of application of hydrogel in the electrode for preparing detection electrocorticogram | |
| CN112932494A (en) | Epidermis dry electrode and manufacturing method thereof and epidermis electric signal acquisition device | |
| CN103293204B (en) | Preparation method of iridium oxide microelectrode controlling electrochemical property by using activated circulation | |
| CN108034972A (en) | A kind of silicon based electrode surface modifying method based on porous gold-Pt nanoparticle | |
| CN209645649U (en) | A kind of functionalization wide cut implantation micro-electrode array | |
| EP3511706B1 (en) | Microelectrode array and manufacturing method therefor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |