CN114635112B - Reactive sputtering ruthenium oxide modified neural electrode array and preparation method thereof - Google Patents
Reactive sputtering ruthenium oxide modified neural 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 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 230000001537 neural effect Effects 0.000 title claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000001301 oxygen Substances 0.000 claims abstract description 40
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 40
- 210000005036 nerve Anatomy 0.000 claims abstract description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052786 argon Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000004544 sputter deposition Methods 0.000 claims description 15
- 229920001721 polyimide Polymers 0.000 claims description 10
- 239000004642 Polyimide Substances 0.000 claims description 7
- 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
- 238000001994 activation Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 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
- 125000004430 oxygen atom Chemical group O* 0.000 abstract 1
- 238000012986 modification Methods 0.000 description 7
- 230000004048 modification Effects 0.000 description 7
- 239000010408 film Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000001727 in vivo Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000003491 array Methods 0.000 description 2
- 210000004556 brain Anatomy 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000000338 in vitro Methods 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
- 210000003710 cerebral cortex Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 230000001788 irregular Effects 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
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
-
- 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
- A61B5/279—Bioelectric electrodes therefor specially adapted for particular uses
- A61B5/291—Bioelectric electrodes therefor specially adapted for particular uses for electroencephalography [EEG]
- A61B5/293—Invasive
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- 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
- A61B5/279—Bioelectric electrodes therefor specially adapted for particular uses
- A61B5/294—Bioelectric electrodes therefor specially adapted for particular uses for nerve conduction study [NCS]
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/04—Coating on selected surface areas, e.g. using masks
- C23C14/042—Coating on selected surface areas, e.g. using masks using masks
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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- A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
- A61B2562/02—Details of sensors specially adapted for in-vivo measurements
- A61B2562/0209—Special features of electrodes classified in A61B5/24, A61B5/25, A61B5/283, A61B5/291, A61B5/296, A61B5/053
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
- A61B2562/12—Manufacturing methods specially adapted for producing sensors for in-vivo measurements
- A61B2562/125—Manufacturing methods specially adapted for producing sensors for in-vivo measurements characterised by the manufacture of electrodes
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Abstract
The invention discloses a nerve electrode array modified by reactive sputtering ruthenium oxide and a preparation method thereof. It comprises the following steps: ruthenium oxide with specific ruthenium and oxygen atom ratio is prepared on the surface of the nerve electrode array by utilizing a reactive sputtering method. Wherein the ruthenium oxide is prepared by reactive sputtering by utilizing argon, oxygen and specific air pressure with specific flow rates. The method and the technological parameters can determine the reactive sputtering condition with good ruthenium oxide adhesion strength, and can obtain good 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 nerve electrode arrays, in particular to a nerve electrode array modified by reactive sputtering ruthenium oxide and a preparation method thereof.
Background
In recent years, the application of an implantable neural electrode array has been rapidly developed, and an invasive electrode directly implants the microelectrode array into the cerebral cortex through surgery and other modes, records the extracellular activity or local field potential close to neurons, obtains accurate brain motor neuron signals, or directly electrically stimulates the neurons, so as to promote the research and decoding of brain related motor information.
The development of the nerve electrode should have technical characteristics required by practical application, including high space-time resolution, high signal-to-noise ratio, biocompatibility, miniaturization and the like. However, the performance of the implanted nerve electrode can be aged slowly in the tissue environment in vivo for a long time, and the problems of rapid increase of the electrode impedance value, falling of the electrode surface packaging material 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 many electrode modification materials, and metal oxides based on redox reactions are one of the more important electrode modification materials.
Through prior art searches, W r. atmaramanni, b. Chakraborty et al, written "Ruthenium oxide based microelectrode arrays for in vitro and in vivo neural recording and stimulation" in Acta Biomaterialia 2020 (ruthenium oxide microelectrode array for in vitro and in vivo nerve recording and stimulation), which describes the feasibility of ruthenium oxide microelectrodes as nerve interfaces. However, this article does not disclose specific implementation steps and parameter tuning methods for the preparation of ruthenium oxide modification.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a reactive sputtering ruthenium oxide modified nerve electrode array facing electrophysiological signal recording and electrical stimulation application and a preparation method thereof.
The invention relates to a nerve electrode array modified by reactive sputtering ruthenium oxide, which comprises the following components: the electrode array to be modified and the reactive sputtering ruthenium oxide material are prepared by a direct current reactive sputtering method in specific flow of argon, oxygen and specific air pressure. The invention is realized by the following technical scheme:
the invention provides a preparation method of a nerve electrode array modified by reactive sputtering ruthenium oxide, which is characterized by comprising the following steps of
The method comprises the following steps:
(1) Firstly, preparing a nerve electrode array to be modified, and exposing an electrode point to be modified in a film mask mode;
(2) Under the conditions that the flow ratio of argon to oxygen is 1:4-3:2, the sputtering pressure is 0.1-1.3 Pa and the current is 0.2-1.1A, the Ru target is directly sputtered on the nerve electrode array to be modified;
(3) And tearing off the film mask to remove the ruthenium oxide with a non-electrode point, thereby obtaining the ruthenium oxide modified nerve electrode array.
In the invention, the implementation method of the step (1) is as follows: using laser to cut the polyimide tape to expose the electrode points as a film mask, and covering the film mask on the nerve electrode array to be modified; or the polyimide tape is covered on the nerve electrode array to be modified, and then the polyimide film in the electrode point region is cut off by laser.
In the invention, in the step (2), the argon flow ranges from 5 to 30 cubic centimeters per minute, and the oxygen flow ranges from 5 to 60 cubic centimeters per minute.
In the invention, in the step (2), the argon flow is in the range of 10-20 cubic centimeters per minute, the oxygen flow is in the range of 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 manufactured by the manufacturing method, and the electrochemical impedance of the nerve electrode array at 1 kHz is 250-1200 ohms after 100 times of electrochemical activation.
In summary, the invention uses argon, oxygen and specific air pressure values with specific flow rates to prepare ruthenium oxide with loose structure, good binding force with a substrate, and good electrochemical property with the element ratio of oxygen to ruthenium close to 2:1, realizes dry mask by a film mask mode, performs dry patterning on the ruthenium oxide, and can obtain better nerve recording or electrical stimulation effect by utilizing the microelectrode modified by sputtering ruthenium oxide with the reaction.
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 under different oxygen flow conditions.
FIG. 3 is a photomicrograph of prepared ruthenium oxide at different oxygen flows.
Fig. 4 is a peak view of XPS test of ruthenium oxide electrode.
FIG. 5 is a graph showing the ratio of elemental components in ruthenium oxide prepared at different oxygen flows.
Detailed Description
The following describes in detail an embodiment of the present invention, which is based on a neural electrode array to be modified, and is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation procedure are given, but the protection scope of the present invention is not limited to the following embodiment.
Example 1
1. Preparation of a neural electrode array:
the polyimide tape was cut using a laser to expose the electrode points and used as a thin film mask to cover the polyimide tape on the nerve electrode array prepared on the 500 μm thick silicon wafer substrate to be modified. In order to obtain higher alignment accuracy, the polyimide tape can be covered on the nerve electrode array to be modified, and then the polyimide film in the electrode point region can be cut off by laser.
The specific preparation process of the reactive sputtered ruthenium oxide comprises the following steps:
firstly, a nerve electrode array needing to sputter ruthenium oxide to modify electrode point areas is placed into a sputtering chamber, and vacuum of the chamber is pumped to 7 multiplied by 10 by using a vacuum pump and a molecular pump -4 Below pascal.
Argon was then introduced and the argon flow was set at 15 cc/min.
Then oxygen is introduced, and different oxygen flow rates are set in sequence, wherein the oxygen flow rate range is 0-60 cubic centimeters per minute. The optimal oxygen flow parameter for this example was 20 cc per minute. The chamber vacuum pressure was regulated to 0.3 pascal.
Setting the current of a direct-current sputtering power supply to be 0.4A, opening a baffle plate of a ruthenium target material, and observing the starting condition.
The sample shutter was opened, the process of reactive sputtering ruthenium oxide was started and the sputtering time was recorded.
And finally, adjusting the current to 0, closing a sputtering power supply, closing a baffle plate, closing oxygen and argon, and ending the reactive sputtering process.
Under the conditions of this example, the ruthenium oxide was prepared by evacuating to 7X 10 -4 The pascal and argon flow are fixed to 15 cubic centimeters per minute, the oxygen flow is 20 cubic centimeters per minute, and sputtering enables the cavity pressure to be 0.3 pascal, so that good electrochemical properties are obtained, and the impedance of the modified microelectrode at 1 kHz is 379.25 ohms after 100 electrochemical activations.
Example 2
The modification effect of ruthenium oxide on the electrode is significantly affected by different oxygen flow rates. According to the invention, the ruthenium oxide adhesion strength is determined to be good according to the multiple test results, and the reactive sputtering condition with good electrochemical properties can be obtained.
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. The pressure is fixed at 0.3 Pa when ruthenium oxide is sputtered, the fixed current is set to be 0.4A, and the oxygen flow is changed to perform magnetron sputtering. It was found that as the oxygen flow increased, the voltage increased first decreased, reaching a maximum value of 572V at an oxygen flow of 20 cc/min.
As shown in FIG. 2, a graph of ruthenium oxide thickness at 10 minutes sputtering time for various oxygen flows is shown. It was found that the thickness of ruthenium oxide increased and decreased with increasing oxygen flow, and that the thickness of ruthenium oxide sputtered for ten minutes at an oxygen flow of 20 cc/min reached 375nm.
As shown in fig. 3, a photomicrograph of the prepared ruthenium oxide at different oxygen flows is shown. Fig. 3 (a) -3 (c) are obtained at oxygen flows of 20, 50, 60 cc/min, respectively. It can be seen that, in fig. 3 (b), 3 (c), the ruthenium oxide on the silicon wafer is in the form of irregular fragments, and the ruthenium oxide is fallen off in a short time after sputtering.
As shown in FIG. 4, the peak value of the XPS test for ruthenium oxide microelectrode with oxygen flow of 20 cubic centimeters per minute is shown. The 1s peak of O, the 3p, 3d peaks of Ru and the 1s peak of C were detected. Table 1 shows the quantitative parameters of XPS test for ruthenium oxide microelectrode with oxygen flow of 20 cc per minute.
As shown in FIG. 5, a graph showing the ratio of elemental components in ruthenium oxide prepared at different oxygen flows is shown. From the data in fig. 5 and tables 1 and 2, it can be found that the oxygen element and ruthenium element composition ratio was 2.01, closest to the oxygen element and ruthenium element composition ratio 2, when the oxygen flow rate was 20 cc/min. Under the condition that the ratio of oxygen element to ruthenium element is 2:1, the valence state of ruthenium is standard positive tetravalent, and the rapid and reversible oxidation-reduction reaction of ruthenium oxide is facilitated. Under this condition, the electrochemical impedance of the electrode at 1 kHz for an oxygen flow of 20 cubic centimeters per minute was 379.2 ohms. Under the condition, the ruthenium oxide has loose structure, good binding force with the substrate and excellent electrode modification effect.
TABLE 1 XPS test table for ruthenium oxide microelectrode with oxygen flow of 20 cc per minute
From the above examples, the present invention utilizes specific flows of argon, oxygen and specific gas pressures to reactively sputter ruthenium oxide, confirming that better electrochemical properties can be obtained. The electrode array can obtain better electrophysiological acquisition and stimulation effects during implantation.
While the present invention has been described in detail through the foregoing description of the preferred embodiment, it should be understood that the foregoing description is not to be considered as limiting the invention. Many modifications and substitutions of the present invention will become apparent to those of ordinary skill in the art upon reading the foregoing. Accordingly, the scope of the invention should be limited only by the attached claims.
Claims (5)
1. The preparation method of the nerve electrode array modified by the reactive sputtering ruthenium oxide is characterized by comprising the following steps of:
(1) Firstly, preparing a nerve electrode array to be modified based on a silicon substrate, and exposing an electrode point to be modified in a film mask mode;
(2) Under the conditions that the flow ratio of argon to oxygen is 1:4-3:2, the sputtering pressure is 0.1-1.3 Pa and the current is 0.2-1.1A, the Ru target is directly sputtered on the nerve electrode array to be modified;
(3) Tearing off the film mask to remove ruthenium oxide with a non-electrode point, so as to obtain a ruthenium oxide modified nerve electrode array; wherein:
the implementation method of the step (1) comprises the following steps: using laser to cut the polyimide tape to expose the electrode points as a film mask, and covering the film mask on the nerve electrode array to be modified; or the polyimide tape is covered on the nerve electrode array to be modified, and then the polyimide film in the electrode point region is cut off by laser.
2. The method according to claim 1, wherein in the step (2), the argon flow is in the range of 5 to 30 cc/min and the oxygen flow is in the range of 5 to 60 cc/min.
3. The method according to claim 1, wherein in the step (2), the flow rate of argon is in the range of 10 to 20 cc/min, the flow rate of oxygen is in the range of 15 to 35 cc/min, and the sputtering current is in the range of 0.3 to 0.8A.
4. The method according to claim 1, wherein in the step (2), the sputtering time is 5 to 20 minutes.
5. A neural electrode array produced according to the production method of claim 1, characterized in that its electrochemical impedance at 1 kHz is in the range of 250-1200 ohms after 100 electrochemical activations.
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Citations (3)
| 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 |
| 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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| TW200742851A (en) * | 2006-05-09 | 2007-11-16 | Univ Nat Yunlin Sci & Tech | Penicillin G biosensors and fabrication method thereof and sensing systems comprising the same |
| GB0620955D0 (en) * | 2006-10-20 | 2006-11-29 | Speakman Stuart P | Methods and apparatus for the manufacture of microstructures |
| KR102382737B1 (en) * | 2015-03-04 | 2022-04-06 | 한국전자통신연구원 | Method for surface modification of neural electrode |
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| 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 |
| 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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