CN114635112A - Reactive sputtering ruthenium oxide modified nerve electrode array and preparation method thereof - Google Patents

Reactive sputtering ruthenium oxide modified nerve electrode array and preparation method thereof Download PDF

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CN114635112A
CN114635112A CN202210183425.5A CN202210183425A CN114635112A CN 114635112 A CN114635112 A CN 114635112A CN 202210183425 A CN202210183425 A CN 202210183425A CN 114635112 A CN114635112 A CN 114635112A
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ruthenium oxide
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CN114635112B (en
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康晓洋
王爱萍
张静
刘鲁生
王君孔帅
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    • A61B5/279Bioelectric electrodes therefor specially adapted for particular uses
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    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract

The invention discloses a reactive sputtering ruthenium oxide modified nerve electrode array and a preparation method thereof. It includes: ruthenium oxide with specific ruthenium and oxygen atom ratio is prepared on the surface of the neural electrode array by a reactive sputtering method. Wherein the ruthenium oxide is prepared by reactive sputtering with specific flow of argon, oxygen and specific gas pressure. The method and the process parameters can determine the reactive sputtering condition with better ruthenium oxide adhesive force strength and can obtain better electrochemical properties. The nerve electrode array modified by the reactive sputtering ruthenium oxide can obtain better electrophysiological signal acquisition and electrical stimulation effects.

Description

Reactive sputtering ruthenium oxide modified neural electrode array and preparation method thereof
Technical Field
The invention relates to the technical field of implanted neural electrode arrays, in particular to a neural electrode array modified by reactive sputtering ruthenium oxide and a preparation method thereof.
Background
In recent years, the application of an implanted nerve electrode array is rapidly developed, and an invasive electrode directly implants a microelectrode array into a cerebral cortex in modes of operation and the like, records extracellular activities or local field potentials close to neurons, obtains accurate brain motor neuron signals, or directly electrically stimulates the neurons, and promotes the research and decoding of brain related motion information.
The development of the above-mentioned neural electrode should have technical characteristics required for practical applications, including high spatial and temporal resolution, high signal-to-noise ratio, biocompatibility, miniaturization, and the like. However, the performance of the implanted nerve electrode slowly ages in the in vivo tissue environment for a long time, and the problems of the sharp increase of the impedance value of the electrode, the falling of the surface packaging material of the electrode and the like are faced, and the performance and the reliability of the electrode array can be effectively improved by carrying out surface modification on the nerve electrode, so that the short-term and long-term usability of the electrode array is enhanced. In order to obtain better electrochemical properties, researchers have developed a number of electrode modification materials, and metal oxides based on redox reactions are one of the more important electrode modification materials.
A search of the prior art has revealed that W R. Atmarani, B. Chakraborty et al, written in Acta biomaterials 2020, "Ruthenium oxide based microelectrodes arrays for in vitro and in vivo neural recording and stimulation" (Ruthenium oxide microelectrode arrays for in vitro and in vivo neural recording and stimulation), introduced the feasibility of Ruthenium oxide microelectrodes as neural interfaces. However, the article does not disclose the specific implementation steps and parameter tuning methods for the modified preparation of ruthenium oxide.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a reactive sputtering ruthenium oxide modified nerve electrode array for electrophysiological signal recording and electrical stimulation application and a preparation method thereof.
The invention discloses a reactive sputtering ruthenium oxide modified nerve electrode array, which comprises: the electrode array to be modified and the reactive sputtering ruthenium oxide are prepared by a direct current reactive sputtering method in specific flow of argon, oxygen and specific gas pressure. The invention is realized by the following technical scheme:
the invention provides a preparation method of a reactive sputtering ruthenium oxide modified nerve electrode array, which is characterized by comprising the following steps of
The method comprises the following steps:
(1) firstly, preparing a neural electrode array to be modified, and exposing electrode points to be modified in a thin film mask mode;
(2) under the conditions of the flow ratio of argon to oxygen being 1:4-3:2, the sputtering pressure range being 0.1-1.3 pascal and the current being 0.2-1.1A, the Ru target is subjected to direct current sputtering on the neural electrode array to be modified;
(3) and tearing off the film mask to remove the ruthenium oxide on the non-electrode points, thereby obtaining the ruthenium oxide modified neural electrode array.
In the invention, the implementation method of the step (1) comprises the following steps: cutting the polyimide adhesive tape by using laser to expose the electrode points as a film mask, and covering the film mask on the neural electrode array to be modified; or firstly covering the polyimide adhesive tape on the neural electrode array to be modified, and then cutting the polyimide film in the power-failure pole area by laser.
In the invention, in the step (2), the flow range of argon is 5-30 cubic centimeters per minute, and the flow range of oxygen is 5-60 cubic centimeters per minute.
In the invention, in the step (2), the flow range of argon is 10-20 cubic centimeters per minute, the flow range of oxygen is 15-35 cubic centimeters per minute, and the sputtering current is 0.3-0.8A.
In the invention, in the step (2), the sputtering time is 5-20 minutes.
The invention also provides a nerve electrode array prepared by the preparation method, wherein the electrochemical impedance of the nerve electrode array at 1 kHz after 100 times of electrochemical activation ranges from 250 ohms to 1200 ohms.
In conclusion, the invention uses argon gas, oxygen gas and specific air pressure value with specific flow rate, can prepare ruthenium oxide with loose structure, good bonding force with the substrate and better electrochemical property, the element ratio of oxygen and ruthenium is close to 2:1, dry masking is realized by a thin film masking mode, dry patterning is carried out on the ruthenium oxide, and the microelectrode modified by utilizing the reactive sputtering ruthenium oxide can obtain better neural recording or electrical stimulation effect.
Drawings
FIG. 1 is a graph of current versus voltage for different oxygen conditions.
FIG. 2 is a graph of the thickness of sputtered ruthenium oxide at different oxygen flow rates.
FIG. 3 is a photomicrograph of prepared ruthenium oxide at various oxygen flow rates.
FIG. 4 is a peak diagram of XPS test of ruthenium oxide electrode.
FIG. 5 is a graph showing the ratios of the elemental components in ruthenium oxide prepared at different oxygen flow rates.
Detailed Description
The following is a detailed description of the embodiments of the present invention, which is based on the neural electrode array to be modified, and is implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of the present invention is not limited to the following embodiments.
Example 1
Firstly, preparing a neural electrode array:
and cutting the polyimide adhesive tape by using laser to expose the electrode points, taking the polyimide adhesive tape as a film mask, and covering the polyimide adhesive tape on a neural electrode array prepared on a silicon wafer substrate with the thickness of 500 microns to be modified. In order to obtain higher alignment precision, a polyimide adhesive tape can be covered on the neural electrode array to be modified, and then the polyimide film in the area of the power failure pole is cut by laser.
The specific preparation process of the reactively sputtered ruthenium oxide is as follows:
firstly, a neural electrode array of an electrode point region needing ruthenium oxide modification by sputtering is put into a sputtering chamber, and the vacuum of the chamber is pumped to 7 multiplied by 10 by using a vacuum pump and a molecular pump-4Pascal or less.
Argon was then introduced, setting the argon flow at 15 cc per minute.
Then introducing oxygen, and setting different oxygen flow rates in sequence, wherein the oxygen flow rate range is 0-60 cubic centimeters per minute. The optimal oxygen flow parameter for this embodiment is 20 cubic centimeters per minute. The vacuum pressure of the conditioning chamber is 0.3 pascal.
The current of the direct current sputtering power supply is set to be 0.4A, the baffle of the ruthenium target is opened, and the glow starting condition is observed.
The sample shutter was opened and the process of reactive sputtering ruthenium oxide was started and the sputtering time was recorded.
And finally, adjusting the current to 0, closing the sputtering power supply, closing the baffle, closing oxygen and argon, and finishing the reactive sputtering process.
Under the conditions of this example, ruthenium oxide was prepared by evacuating to 7X 10-4The better electrochemical property is obtained under the conditions that the flow of Pascal and argon gas is fixed to be 15 cubic centimeters per minute, the flow of oxygen is 20 cubic centimeters per minute, the pressure of a cavity is 0.3 Pascal through sputtering, and the impedance of the modified microelectrode at 1 kHz is 379.25 ohms after 100 times of electrochemical activation.
Example 2
Since different oxygen flow rates can significantly affect the modification effect of ruthenium oxide on the electrode. According to the invention, the reactive sputtering condition that the ruthenium oxide has better adhesive strength and can obtain better electrochemical property is determined according to the test results.
As shown in fig. 1, the graph shows the variation trend of the sputtering voltage under the conditions of different oxygen and the same current. When sputtering ruthenium oxide, the pressure is fixed at 0.3 Pa, the fixed current is set at 0.4A, and the oxygen flow is changed to carry out magnetron sputtering. It was found that as the oxygen flow rate increased, the voltage increased and decreased, reaching a maximum of 572V at an oxygen flow rate of 20 cc per minute.
As shown in FIG. 2, the thickness of the ruthenium oxide is plotted for different oxygen flow rates and 10 minutes sputtering time. It was found that the thickness of the ruthenium oxide first increased and decreased with increasing oxygen flow, and reached 375nm for ten minutes of sputtering at an oxygen flow of 20 cc per minute.
As shown in fig. 3, photomicrographs of the prepared ruthenium oxide are shown for different oxygen flow rates. Fig. 3 (a) -3 (c) are obtained with oxygen flow rates of 20, 50, 60 cubic centimeters per minute, respectively. It can be seen that FIGS. 3 (b), 3(c) show that the ruthenium oxide on the silicon wafer is in a fractal shape, and the ruthenium oxide exfoliation phenomenon occurs in a short time after sputtering the ruthenium oxide.
As shown in FIG. 4, it is a graph of XPS test peak of ruthenium oxide microelectrode with oxygen flux of 20 cubic centimeters per minute. The 1s peak of O, the 3p and 3d peaks of Ru and the 1s peak of C were detected. Table 1 shows the quantitative parameters of the XPS test of a ruthenium oxide microelectrode with an oxygen flux of 20 cc/min.
As shown in FIG. 5, a graph of the ratio of the elemental components in ruthenium oxide prepared at different oxygen flow rates is shown. From the data in fig. 5 and tables 1 and 2, it can be seen that when the oxygen flow rate is 20 cc/min, the elemental oxygen and ruthenium composition ratio is 2.01, which is closest to the elemental oxygen and ruthenium composition ratio 2. Under the condition that the proportion of oxygen element and ruthenium element is 2:1, the valence state of ruthenium is standard positive quadrivalence, which is beneficial to the rapid and reversible redox reaction of ruthenium oxide. Under this condition, the electrochemical impedance of the electrode at 1 kHz, with an oxygen flow rate of 20 cubic centimeters per minute, was 379.2 ohms. Under the condition, the ruthenium oxide has loose structure, good bonding force with the substrate and excellent electrode modification effect.
TABLE 1 XPS test chart for ruthenium oxide microelectrode with oxygen flow of 20 cubic centimeters per minute
Figure 320533DEST_PATH_IMAGE001
From the above examples, it can be seen that the present invention utilizes a specific flow of argon, oxygen, and a specific gas pressure to reactively sputter ruthenium oxide, confirming that better electrochemical properties can be obtained. The electrode array can obtain better electrophysiological acquisition and stimulation effects when being implanted.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.

Claims (6)

1. A preparation method of a reactive sputtering ruthenium oxide modified nerve electrode array is characterized by comprising the following steps:
(1) firstly, preparing a silicon substrate-based neural electrode array to be modified, and exposing electrode points to be modified in a thin film mask mode;
(2) under the conditions of the flow ratio of argon to oxygen being 1:4-3:2, the sputtering pressure range being 0.1-1.3 pascal and the current being 0.2-1.1A, the Ru target is subjected to direct current sputtering on the neural electrode array to be modified;
(3) and tearing off the film mask to remove the ruthenium oxide on the non-electrode points, thereby obtaining the ruthenium oxide modified neural electrode array.
2. The method according to claim 1, wherein the step (1) is performed by: cutting the polyimide adhesive tape by using laser to expose the electrode points as a film mask, and covering the film mask on the neural electrode array to be modified; or firstly covering the polyimide adhesive tape on the neural electrode array to be modified, and then cutting the polyimide film in the power-failure pole area by laser.
3. The method according to claim 1, wherein in the step (2), the flow rate of argon gas is in the range of 5 to 30 cubic centimeters per minute and the flow rate of oxygen gas is in the range of 5 to 60 cubic centimeters per minute.
4. The method of claim 1, wherein in the step (2), the argon flow rate is in a range of 10 to 20 cubic centimeters per minute, the oxygen flow rate is in a range of 15 to 35 cubic centimeters per minute, and the sputtering current is in a range of 0.3 to 0.8A.
5. The production method according to claim 1, wherein in the step (2), the sputtering time is 5 to 20 minutes.
6. The neural electrode array prepared by the preparation method according to claim 1, wherein the electrochemical impedance at 1 kHz ranges from 250 ohms to 1200 ohms after 100 times of electrochemical activation.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5585776A (en) * 1993-11-09 1996-12-17 Research Foundation Of The State University Of Ny Thin film resistors comprising ruthenium oxide
JPH09331034A (en) * 1996-06-07 1997-12-22 Sharp Corp Oxide electrode film forming method
US20070261955A1 (en) * 2006-05-09 2007-11-15 National Yunlin University Of Science And Technology Ruthenium oxide electrodes and fabrication method thereof
US20110207328A1 (en) * 2006-10-20 2011-08-25 Stuart Philip Speakman Methods and apparatus for the manufacture of microstructures
US20160258070A1 (en) * 2015-03-04 2016-09-08 Electronics And Telecommunications Research Institute Method for surface-modifying neural electrode
CN109659146A (en) * 2018-12-18 2019-04-19 清华大学 Three-dimensional micro-pillar array active electrode and preparation method based on tubular metal oxide

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5585776A (en) * 1993-11-09 1996-12-17 Research Foundation Of The State University Of Ny Thin film resistors comprising ruthenium oxide
JPH09331034A (en) * 1996-06-07 1997-12-22 Sharp Corp Oxide electrode film forming method
US20070261955A1 (en) * 2006-05-09 2007-11-15 National Yunlin University Of Science And Technology Ruthenium oxide electrodes and fabrication method thereof
US20110207328A1 (en) * 2006-10-20 2011-08-25 Stuart Philip Speakman Methods and apparatus for the manufacture of microstructures
US20160258070A1 (en) * 2015-03-04 2016-09-08 Electronics And Telecommunications Research Institute Method for surface-modifying neural electrode
CN109659146A (en) * 2018-12-18 2019-04-19 清华大学 Three-dimensional micro-pillar array active electrode and preparation method based on tubular metal oxide

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