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 PDFInfo
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- 229910001925 ruthenium oxide Inorganic materials 0.000 title claims abstract description 48
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000005546 reactive sputtering Methods 0.000 title claims abstract description 18
- 210000005036 nerve Anatomy 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000001301 oxygen Substances 0.000 claims abstract description 38
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 38
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000001537 neural effect Effects 0.000 claims abstract description 25
- 229910052786 argon Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000007789 gas Substances 0.000 claims abstract description 6
- 238000004544 sputter deposition Methods 0.000 claims description 19
- 229920001721 polyimide Polymers 0.000 claims description 11
- 239000004642 Polyimide Substances 0.000 claims description 8
- 239000002390 adhesive tape Substances 0.000 claims description 8
- 239000010408 film Substances 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 229910001882 dioxygen Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052707 ruthenium Inorganic materials 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 230000000638 stimulation Effects 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 125000004430 oxygen atom Chemical group O* 0.000 abstract 1
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 5
- 238000003491 array Methods 0.000 description 3
- 238000001727 in vivo Methods 0.000 description 3
- 210000004556 brain Anatomy 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000000338 in vitro Methods 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 210000002569 neuron Anatomy 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 210000003710 cerebral cortex Anatomy 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 239000002421 finishing Substances 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 210000002161 motor neuron Anatomy 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/24—Detecting, measuring or recording bioelectric or biomagnetic signals of the body or parts thereof
- A61B5/25—Bioelectric electrodes therefor
- A61B5/263—Bioelectric electrodes therefor characterised by the electrode materials
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- A—HUMAN NECESSITIES
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- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
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- A61B5/25—Bioelectric electrodes therefor
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- C23C14/00—Coating 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
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
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)
| 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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Patent Citations (6)
| 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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