CN116019455A - Flexible high-density scalp electroencephalogram electrode and preparation method thereof - Google Patents
Flexible high-density scalp electroencephalogram electrode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a flexible high-density scalp electroencephalogram electrode and a preparation method thereof, wherein the flexible high-density scalp electroencephalogram electrode comprises: the carrier and N tantalum wires are formed by solidifying sensitive materials, and the method for preparing the sensitive materials comprises the following steps: uniformly mixing PDMS and an aqueous solution of tetrachloroauric acid, keeping the temperature at 70-80 ℃ for 1-1.5 h, reducing the tetrachloroauric acid into gold particles or gold trichloride, cooling to room temperature, adding a hybrid, and performing ultrasonic treatment to obtain a sensitive material, wherein the hybrid is a mixture of a carbon conductive material and titanium dioxide nano powder. The sensitive material has good flexibility, can not cause a tested person to feel uncomfortable, and the flexible high-density scalp electroencephalogram electrode is matched with the conductive liquid to enable the acquisition of the electroencephalogram signal in the hair area to be more stable, convenient and quick.
Description
Technical Field
The invention belongs to the technical field of scalp electroencephalogram electrodes, and particularly relates to a flexible high-density scalp electroencephalogram electrode and a preparation method thereof.
Background
The brain, which is the central nervous system, is the most complex system of structures and functions known to humans at present. Because of its important significance in the fields of life science, medical health, etc., human research on the brain has never been stopped. The acquisition and analysis of electrical signals generated in the brain is an effective means of studying the brain. The electrical signals in the brain can reflect the health and state of people, and are important parameters for treating brain diseases, and scalp electroencephalogram attracts many scientists to explore due to the characteristics of no damage, convenience and low cost.
Electroencephalogram (EEG) is one of the most commonly used and most economical non-invasive means of brain wave detection. The electroencephalogram has high time resolution and has important value in the aspect of treating epilepsy and mental diseases. Electroencephalogram can be classified into scalp electrode electroencephalogram and intracranial electrode electroencephalogram according to whether the electrodes are placed in the cranium or outside the cranium. Electroencephalogram, like electrocardiogram, is the recording of bioelectrical activity by means of instruments. Scalp electrode electroencephalogram is a graph obtained by placing electrodes at specific positions of scalp, collecting microvoltage signals generated by the activity of synchronous neurons in the brain, amplifying and recording, and is spontaneous and rhythmic electric activity of brain cell groups recorded by the electrodes.
Along with the continuous development of electroencephalogram application, the requirements on an electroencephalogram acquisition electrode are also higher and higher. Two main categories can be distinguished depending on whether the electrode is invasive: non-invasive electrode and invasive electrode. Common non-invasive electrodes are scalp EEG recording electrodes (Ag/AgCl electrodes); the invasive electrode comprises a metal microfilament electrode, a glass microelectrode, a silicon-based microelectrode and a brain cortex electric signal recording electrode. Invasive electrodes are often used to collect brain signals because they cause damage to the subject.
Non-invasive electrodes are classified into dry electrodes, wet electrodes, and semi-dry electrodes, and have various forms of existence, including single-channel electrodes, high-density electrodes, brush-like semi-dry electrodes, and the like. Because the brain may need to work cooperatively between different regions when subjected to sensory stimuli or cognitive activities, the information of a single local region may not describe the entire perception pattern. There is therefore a need for research that extends from single-channel to multi-channel electroencephalogram signals. High density electrodes have been developed that contain multiple channels, principally to collect more independently valid signals in a limited range of space. The more channels, the more information is obtained. The high-density acquisition has important significance for exploring the law of potential change in brain and researching brain mechanism and brain-computer interface field. With the continuous and intensive research on high-density electrodes, fine motion regulation and control can be performed subsequently through the contraction motions of local brain channel areas and nerve control muscle tissues. However, the rigid material of the existing non-invasive high-density electrode cannot be tightly attached to the head, especially the hair area, is easy to damage the skin, has low signal-to-noise ratio and overlarge impedance, and is not beneficial to signal acquisition.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a flexible high-density scalp electroencephalogram electrode, which uses Polydimethylsiloxane (PDMS) as a flexible material, adds a carbon conductive material to construct a conductive net, then adds titanium dioxide nano powder and tetrachloroauric acid, reduces polarization potential by utilizing the wide negative potential window advantage of the titanium dioxide nano powder, improves scalp affinity at the same time, reduces gold nano particles by utilizing tetrachloroauric acid to improve conductivity and electron capturing capability, and performs local high-density signal acquisition through an N channel. The flexible high-density scalp electroencephalogram electrode has the advantages of stable signals, high density, flexibility and comfort.
Another object of the invention is to provide a method for preparing the flexible high-density scalp electroencephalogram electrode.
Another object of the present invention is to provide a conductive liquid, and a flexible high-density scalp electroencephalogram electrode can quickly adjust impedance to be stable in combination with the conductive liquid.
The aim of the invention is achieved by the following technical scheme.
A flexible high density scalp electroencephalogram electrode comprising: a carrier and N tantalum filaments, the carrier comprising: the device comprises a substrate and N claw posts connected to the bottom surface of the substrate, wherein each claw post penetrates through one tantalum wire, the bottom end of each tantalum wire is flush with the bottom surface of each claw post and used for collecting ions to form micro-current, the top end of each tantalum wire is located above the substrate and used for being connected with an electrode wire, the carrier is formed by solidifying a sensitive material, and the method for preparing the sensitive material comprises the following steps: uniformly mixing PDMS and an aqueous solution of tetrachloroauric acid, keeping the temperature at 70-80 ℃ for 1-1.5 h, reducing the tetrachloroauric acid into gold particles or gold trichloride, cooling to room temperature, adding a hybrid, and performing ultrasonic treatment to obtain a sensitive material, wherein the hybrid is a mixture of a carbon conductive material and titanium dioxide nano powder, and the mass ratio of the tetrachloroauric acid, the carbon conductive material, the titanium dioxide nano powder and the PDMS in the aqueous solution of tetrachloroauric acid is (0.000003-0.000006): (0.5-3): (0.5-2.5): (92-99) according to the mass parts.
In the technical scheme, the PDMS is formed by mixing a silica gel elastomer substrate and a silica gel elastomer curing agent, and the ratio of the silica gel elastomer substrate to the silica gel elastomer curing agent is (9-11): 1 according to the mass parts.
In the above technical solution, the carbon conductive material is a multi-walled carbon nanotube or a single-walled carbon nanotube.
In the technical proposal, the concentration of the tetrachloroauric acid in the tetrachloroauric acid aqueous solution is 10 -6 ～10 -4 mol/L。
In the above technical solution, n=19.
In the technical scheme, the length of the tantalum wire is 5-6 cm, the diameter of the tantalum wire is 0.2-0.6 mm, the claw columns are round tables which taper from top to bottom, the height of each claw column is 3-6 mm, the diameter of the bottom surface of each claw column is 1-1.5 mm, the diameter of the top surface of each claw column is 2-2.5 mm, the axial distance between every two adjacent claw columns is 2.5-4 mm, the base is cylindrical, the diameter of the base is 15-20 mm, and the height of the base is 6-10 mm.
The preparation method of the flexible high-density scalp electroencephalogram electrode comprises the following steps:
1) Pouring the sensitive material into a mold twice, and vacuumizing for 10-15 min after each pouring;
in the step 1), vacuum is pumped to below-0.08 MPa.
In the step 1), the mass ratio of the sensitive materials poured into the mould in two times is (2-3): 5.
2) Inserting N tantalum wires into the sensitive material, keeping the temperature at 60-80 ℃ for 2-5 hours to solidify the sensitive material to form the carrier, and taking out the flexible high-density scalp electroencephalogram electrode from the die.
A conductive liquid is prepared by mixing sodium carboxymethylcellulose (CMC) and saturated saline water, wherein the ratio of the mass parts of the sodium carboxymethylcellulose to the volume parts of the saturated saline water at 25 ℃ is (1-1.1): 20, the unit of the mass parts is g, and the unit of the volume parts is mL.
In the technical scheme, the conductive liquid is matched with the flexible high-density scalp electroencephalogram electrode.
The beneficial effects of the invention are as follows:
1. the sensitive material disclosed by the invention is based on polydimethylsiloxane, has good flexibility, and can not cause uncomfortable feeling to a tested person;
2. the titanium dioxide nano powder used in the sensitive material has excellent chemical stability, thermal stability and antibacterial property; gold particles are gradually reduced by the tetrachloroauric acid in the two heating processes, so that the electron capturing capability of the sensitive material is improved;
3. the flexible high-density scalp electroencephalogram electrode is more stable, convenient and quick in acquisition of electroencephalogram signals in the hair area due to the high density and the conductive liquid;
4. the circuit adopts an N-lead mode to reduce scalp interface impedance, and the carrier is an insulator when not electrified and is a conductor with smaller impedance when electrified due to the special structure of the circuit. The advantages in performance are obvious, and the correlation degree with the traditional wet electrode is high.
5. The conductive liquid is pasty and not easy to flow, and can be well attached to the flexible high-density scalp electroencephalogram electrode during testing, thereby facilitating the test of electroencephalogram signals.
Drawings
FIG. 1 is a photograph of a flexible high density scalp electroencephalogram electrode of the present invention;
fig. 2 is a bottom view (numbered) of the carrier;
FIG. 3 is a cross-sectional view of a flexible high density scalp electroencephalogram electrode;
FIG. 4 is a photograph of a flexible high density scalp electroencephalogram (above the eyebrows) when tested;
FIG. 5 is a graph showing the impedance of a conventional wet electrode-Ag/AgCl electrode and a flexible high density scalp electroencephalogram electrode;
FIG. 6 is a diagram of an original signal waveform (blink), with a depression being a blink waveform;
FIG. 7 is a diagram of the original signal waveform (bite), with the saw tooth shape being a bite waveform;
FIG. 8 is a plot of the correlation of the antenna of a flexible high density scalp electroencephalogram electrode with the blink signal of a conventional wet electrode-Ag/AgCl electrode;
FIG. 9 is a plot of the correlation of the antenna of a flexible high density scalp electroencephalogram electrode with the tooth biting signal of a conventional wet electrode-Ag/AgCl electrode;
FIG. 10 is a photograph (occipital region) of a flexible high density scalp electroencephalogram electrode test;
FIG. 11 is a graph showing the impedance of a conventional wet electrode-Ag/AgCl electrode and a flexible high density scalp electroencephalogram electrode;
fig. 12 is a waveform diagram of an original signal (open eye);
FIG. 13 is a graph showing correlation of the eye opening and closing signals of the antennae of the flexible high-density scalp electroencephalogram electrode and the conventional wet electrode-Ag/AgCl electrode;
FIG. 14 is a graph of signal to noise ratio of each antenna of a flexible high density scalp electroencephalogram electrode (the "I" shaped line in the figure is an error bar);
fig. 15 is a spectrum diagram of the flexible high-density scalp electroencephalogram electrode in the eye-closing and eye-opening state of the subject, XC represents the spectrum in the eye-closing state (a relatively convex line in the figure), XO represents the spectrum in the eye-opening state (a relatively gentle line in the figure), and x=an integer of 1 to 19, which in turn represent the antennas numbered 1 to 19 in fig. 2;
FIG. 16 is a correlation of the open and closed eye signals of the flexible high density scalp electroencephalogram electrode in example 2 with the conventional wet electrode-Ag/AgCl electrode;
FIG. 17 is a graph showing the signal-to-noise ratio of the antennae of the flexible high density scalp electroencephalogram electrode of example 2 (the "I" shaped line is an error bar);
fig. 18 is a spectrum diagram of the flexible high-density scalp electroencephalogram electrode in example 2 in the eye-closing and eye-opening states of the subject, XC represents the spectrum in the eye-closing state (the relatively convex line in the figure), XO represents the spectrum in the eye-opening state (the relatively gentle line in the figure), x=an integer of 1 to 19, and the integers in x=1 to 19 sequentially represent the antennas numbered 1 to 19 in fig. 2;
FIG. 19 is a plot of the correlation between the antennae of the flexible high density scalp electroencephalogram electrode;
FIG. 20 is an interface contact resistance of a planar electrode prepared from the sensitive material obtained in example 1 and a planar electrode prepared from the sensitive material obtained in comparative example 1, respectively, with a saturated aqueous sodium chloride solution;
FIG. 21 is a photograph of a bend formed by curing the sensitive material of example 1 and comparative example 1 into a sheet;
fig. 22 is a photograph showing the discs respectively pressed in a pair of rollers.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
The sources of the drugs involved in the examples below are as follows:
1. multiwall carbon nanotubes, manufacturer: shenzhen City Tuling evolution technology Co., ltd;
2. single-walled carbon nanotubes, manufacturer: nanjing Xianfeng nanomaterials technologies Co., ltd;
3. titanium dioxide nanopowder, manufacturer: gaussda nanomaterial plant Co.Ltd in four-plain;
4. tetrachloroaurate, manufacturer: alfa Aesar (USA);
5. sodium carboxymethylcellulose, manufacturer: tianjin Xingxing institute for fine chemical industry;
6. the silicone elastomer substrate and silicone elastomer curing agent were purchased from dakangnin PDMS, model: 184;
7. conductive paste, manufacturer: compumedics (USA);
the sources of the instruments involved in the examples below are as follows:
1. vacuum drying box: product model: DZF-6050, vendor name: shanghai-Heng science instruments Co., ltd;
2. constant temperature magnetic stirrer: product model B11-2, vendor name: shanghai Sele instruments Co Ltd;
3. ultrasonic cleaner: product model: KQ2200E.
The preparation method of the aqueous solution of the tetrachloroauric acid comprises the following steps: firstly, putting a 25mL beaker on a balance for zero clearing, then quickly weighing 0.3397g of tetrachloroauric acid by a spoon, then pouring the tetrachloroauric acid into a 10mL volumetric flask, adding absolute ethyl alcohol for constant volume to obtain 0.1mol/L of tetrachloroauric acid aqueous solution, and diluting to 10 -4 mol/L。
Before using, the tantalum wire is polished by 220-mesh (68 μm) fine sand paper, surface oxides and dirt are removed, the tantalum wire is sequentially cleaned by ultrasonic in 99.7wt% alcohol and ultrapure water for 5min, and the tantalum wire is naturally dried.
The conductive liquid in the following examples is formed by mixing sodium carboxymethylcellulose (CMC) and saturated saline at 25 ℃, wherein the ratio of the mass parts of the sodium carboxymethylcellulose to the volume parts of the saturated saline is 1.1:20, the unit of the mass parts is g, and the unit of the volume parts is mL. Preparing a conductive liquid: sodium carboxymethylcellulose (CMC) was weighed by an electronic balance, poured into a beaker, then saturated saline was added, stirred well, added to a rotor and placed on a magnetic stirrer at 80r/s for 5 hours.
Example 1
As shown in fig. 1, a flexible high density scalp electroencephalogram electrode, comprising: carrier and N tantalum silk, the carrier includes: the substrate and connect N claw posts on the substrate bottom surface, N=19, N claw posts's arrangement is as shown in fig. 2, and N claw posts divide into six rows, and six rows claw posts are from top to bottom every claw post's number in proper order: the claw posts in the adjacent rows are staggered from each other, wherein the claw posts are 3, 4, 5, 4 and 3. As shown in fig. 3, each claw column passes through a tantalum wire, wherein the bottom end of each tantalum wire is flush with the bottom surface of the claw column and is used for collecting ions to form micro-current, the top end of the tantalum wire is positioned above the substrate and is used for being connected with electrode wires, one tantalum wire is connected with one electrode wire, the N electrode wires are numbered and are connected with a signal acquisition device, the number is shown in fig. 2, the carrier is formed by solidifying a sensitive material, and the method for preparing the sensitive material comprises the following steps: uniformly mixing PDMS and an aqueous solution of tetrachloroauric acid, keeping the temperature at 78 ℃ for 1.5 hours, cooling to the room temperature of 20-25 ℃ to reduce the tetrachloroauric acid into gold particles or gold trichloride, adding a hybrid, and performing ultrasonic treatment for 5 minutes to obtain a sensitive material, wherein the hybrid is a mixture of a carbon conductive material and titanium dioxide nano powder, and the mass ratio of the tetrachloroauric acid, the carbon conductive material, the titanium dioxide nano powder and the PDMS in the aqueous solution of tetrachloroauric acid is 0.000003:1.7:2.1:96.17.
The PDMS is formed by mixing a silica gel elastomer substrate and a silica gel elastomer curing agent, wherein the ratio of the silica gel elastomer substrate to the silica gel elastomer curing agent is 10:1, the carbon conductive material is a multi-wall carbon nano tube, and the concentration of tetrachloroauric acid in a tetrachloroauric acid aqueous solution is 10 percent -4 mol/L。
The length of the tantalum wire is 5cm, and the diameter of the tantalum wire is 0.2mm; the claw post is the round platform of gradual taper from top to bottom, and the height of claw post is 6mm, and the circular diameter of bottom surface of claw post is 1.5mm, and the circular diameter of top surface of claw post is 2.5mm, and the axle center distance of adjacent claw post is 3.5mm, and the base is cylindrical, and the diameter of base is 20mm, and the height of base is 10mm.
The preparation method of the flexible high-density scalp electroencephalogram electrode comprises the following steps:
1) Pouring the sensitive materials into a mold twice, pouring the sensitive materials into the mold sequentially with the mass ratio of 2:5, and vacuumizing to-0.08 Mpa and maintaining for 10min after each pouring;
2) Inserting N tantalum wires into the sensitive material, keeping the temperature at 72 ℃ for 2 hours to solidify the sensitive material to form a carrier, and taking out the flexible high-density scalp electroencephalogram electrode from the die.
The flexible high-density scalp electroencephalogram electrode is adopted for testing: three conventional wet electrodes, ag/AgCl electrodes (produced by Beijing Qing Beijing electronic technology Co.), scrub, conductive paste, dust-free cloth, medical adhesive tape and conductive liquid were prepared, and the equipment used for signal acquisition was 32-lead electroencephalogram acquisition equipment of the model Greal, neuroscan company, australia.
(1) Collecting brain electrical signals of blinks and bites in hairless area
The impedance, signal waveform and correlation between the analysis electrodes of the flexible high-density scalp electroencephalogram electrode are observed by taking the conventional wet electrode-Ag/AgCl electrode as a reference. Firstly, wiping mastoid behind ears of a tested person by using a small amount of abrasive paste which is dipped by dust-free cloth, wherein the abrasive paste has the function of removing stratum corneum on the surfaces of mastoid, respectively beating 0.2mL of conductive paste on two traditional wet electrode-Ag/AgCl electrodes to fill recesses of the traditional wet electrode-Ag/AgCl electrodes, and respectively fixing the recesses at the positions of mastoid behind the two ears by using a medical adhesive tape, wherein one of the positions is used as a reference electrode, and the other position is used as a grounding electrode. Two adjacent positions above the eyebrow of the tested person are selected and wiped by using scrub cream to form a first area and a second area, a third traditional wet electrode-Ag/AgCl electrode is sprayed with an equivalent amount of conductive paste to be placed in the first area, and a flexible high-density scalp electroencephalogram electrode is dipped with conductive liquid to be placed in the second area and fixed by using a head band, as shown in fig. 4. Test with Grael EEG equipment and Curry 8 software. The contact end of each tantalum wire of the flexible high-density scalp electroencephalogram electrode with the skin is an antenna, the antenna is respectively and independently connected with the great EEG equipment, the impedance value is shown in figure 5, 1-19 represent N antennae of the flexible high-density scalp electroencephalogram electrode, and 27 represents a traditional wet electrode-Ag/AgCl electrode; the original waveform of the blink is shown in fig. 6, and the original waveform of the bite is shown in fig. 7. On the premise that the contact area of each antenna of the flexible high-density scalp electroencephalogram electrode and the scalp is less than three percent of the contact area of the traditional wet electrode-Ag/AgCl electrode and the scalp, the impedance of each antenna of the flexible high-density scalp electroencephalogram electrode is close to the impedance of the traditional wet electrode-Ag/AgCl electrode.
Processing brain electrical signals acquired by the flexible high-density scalp electroencephalogram electrode by MATLAB, and then drawing by using Origin2018 software, wherein the correlation degree of each antenna of the flexible high-density scalp electroencephalogram electrode and blink signals of the traditional wet electrode-Ag/AgCl electrode is about 97%, as shown in figure 8; the correlation degree of each antenna of the flexible high-density scalp electroencephalogram electrode and the tooth biting signal of the conventional wet electrode-Ag/AgCl electrode is about 97%, as shown in fig. 9.
(2) Collecting eye brain electrical signals for opening and closing pillow area
Firstly, a small amount of scrub paste is dipped with dust-free cloth to wipe the mastoid behind the ears of a tested person, conductive paste is respectively applied on two traditional wet electrode-Ag/AgCl electrodes to fill recesses of the wet electrode-Ag/AgCl electrodes, and the wet electrode-Ag/AgCl electrodes are respectively fixed at the mastoid behind the ears by using medical adhesive tapes, wherein one of the wet electrode-Ag/AgCl electrodes is used as a reference electrode, and the other wet electrode-Ag/AgCl electrode is used as a grounding electrode. Selecting two adjacent positions in the pillow area of the tested person, wiping the two adjacent positions with scrub paste to form a first area and a second area, beating a third traditional wet electrode-Ag/AgCl electrode with an equal amount of conductive paste, placing the third traditional wet electrode-Ag/AgCl electrode in the first area, dipping a flexible high-density scalp electroencephalogram electrode into conductive liquid, placing the flexible high-density scalp electroencephalogram electrode in the second area, fixing the flexible high-density scalp electroencephalogram electrode by a head band, fixing the traditional wet electrode-Ag/AgCl electrode at a position about 3cm above the flexible high-density scalp electroencephalogram electrode by a head net, and wearing the flexible high-density scalp electroencephalogram electrode as shown in a figure 10.
During testing, conducting liquid is smeared on the bottom surface of the claw pole, the impedance value of each channel of the flexible high-density scalp electroencephalogram electrode is reduced to about 30k omega-50 k omega by slightly adjusting the distance between the scalp and the bottom surface of the claw pole, signal acquisition is carried out after the impedance value is relatively stable, the adjustment time is within half an hour, the impedance values are shown in fig. 11, 1-19 respectively represent N antennae of the flexible high-density scalp electroencephalogram electrode, and 27 represents a traditional wet electrode-Ag/AgCl electrode. As shown in fig. 12, the original waveform of the open-eye is a waveform of a large and sparse amplitude, in which an alpha wave appears when the left side of the vertical line in fig. 12 is the eye-closed state (the right side is the eye-open state) of the subject. After the acquired brain electrical signals are processed by MATLAB, the original graph is used, and the correlation degree between each antenna of the flexible high-density scalp brain electrical electrode and the open-close eye signals of the traditional wet electrode-Ag/AgCl electrode can reach 98%, as shown in figure 13. The signal to noise ratio of each antenna of the flexible high-density scalp electroencephalogram electrode can reach about 7.6dB, as shown in figure 14.
The tested person is kept in a eye closing state or an eye opening state, the electroencephalogram signals collected by the tested person in the eye closing state and the eye opening state are processed by using Origin2018 software from time domain to frequency domain, and the spectrogram of each antenna of the flexible high-density scalp electroencephalogram electrode is shown in figure 15. The human can generate 8-13 Hz alpha rhythm in the awake, eye-closing and calm states, and the amplitude of the alpha rhythm can be used as a standard for measuring the electrode preference of the brain electricity as shown by the peak value in figure 15. As shown in fig. 15, the amplitude of the alpha wave measured by the flexible high-density scalp electroencephalogram electrode of the subject in the eye-closed state is about 6 μv.
In the test, if the conductive liquid is not smeared on the bottom surface of the claw pole, the impedance of the flexible high-density scalp electroencephalogram electrode is more than 250k omega, and signal acquisition cannot be carried out. If physiological saline is smeared on the bottom surface of the claw pole, the impedance is also reduced, but the physiological saline has strong fluidity, and the acquisition of the brain electrical signals is inconvenient. If the conductive paste is applied to the bottom surface of the claw beam, the final impedance value can be reduced to 30k omega-50 k omega, but the impedance reduction time is slow, about 40 minutes.
Comparative example 1
A flexible comb-shaped semi-dry electrode, which is disclosed in the specification example 3 of the publication No. CN 112967832A.
The flexible high density scalp electroencephalogram electrode obtained in example 1 and the flexible comb-shaped semi-dry electrode obtained in comparative example 1 were compared.
The flexible comb-shaped semi-dry electrode is in large-area contact with the skin by 19 claw column bottoms, the impedance obtained by the 19 claw column bottoms is about 5-10 kΩ, and the calculated resistance per square centimeter is about 14kΩ; the contact area of the bottom surface of each claw column of the flexible high-density scalp electroencephalogram electrode and the skin is less than three percent of the contact area of the flexible comb electrode and the skin, the impedance average of the flexible high-density scalp electroencephalogram electrode is about 30kΩ, and the resistance of each claw column bottom surface of the flexible high-density scalp electroencephalogram electrode is about 4.7kΩ; from this, it can be seen that the sensitive material in example 1 has a technical effect of reducing resistance compared to the sensitive material in comparative example 1.
The correlation degree between the flexible comb-shaped semi-dry electrode obtained in the comparative example 1 and the traditional wet electrode-Ag/AgCl electrode is about 98%; the correlation degree between each antenna of the flexible high-density scalp electroencephalogram electrode obtained in the embodiment 1 and the conventional wet electrode-Ag/AgCl electrode is about 98%, and the correlation degree between each antenna of the flexible high-density scalp electroencephalogram electrode obtained by processing the acquired signals by MATLAB and then plotting the acquired signals by Origin2018 is up to 99%, as shown in fig. 19.
The sensitive material in example 1 and the sensitive material in example 2 in CN112967832a were each made into a planar electrode comprising: a sector column body formed by curing a sensitive material at 72 ℃ for 2 hours is formed, a tantalum wire with the diameter of 0.6mm is inserted into the sensitive material before curing, the thickness of the sector column body is 3mm, the sector radius of the sector column body is 10mm, the central angle of the sector column body is 90 degrees, the length of the tantalum wire is 5cm, one end of the tantalum wire is bent into a circle with the diameter of 2.2mm, and then the end with the circle of the tantalum wire is inserted into the sector column body. Preparation of the planar electrode from the sensitive Material in example 1 was Au-TiO 2 CNT@PDMS planar electrode made of sensitive material of example 2 in CN112967832A is Cu-TiO 2 -CNT@PDMS。
Testing of Au-TiO by electrochemical workstation and three electrode system 2 -CNT@PDMS and Cu-TiO 2 -contact resistance of cnt@pdms at the interface with 25 ℃ saturated aqueous sodium chloride solution, respectively. The three-electrode system is a counter electrode, a reference electrode and a working electrode, wherein the counter electrode is a platinum sheet electrode, the reference electrode is a silver-silver chloride electrode, the working electrode is a plane electrode, and the three-electrode system is immersed in a saturated sodium chloride aqueous solution at 25 ℃, and the test result is shown in figure 20. As can be seen from fig. 20, the interface contact resistance of the working electrode prepared from the sensitive material obtained in example 1 was smaller than that of the working electrode prepared from the sensitive material obtained in example 2 in CN112967832 a.
The sensitive materials of example 1 and comparative example 1 were cured at 72℃for 2 hours to form a sheet of 1cm in length, 5mm in width and 1mm in thickness, respectively, and the degree of bending was observed as shown in FIG. 21, in which the sensitive material of example 1 was shown on the left and the sensitive material of comparative example 1 on the right. It can be seen from the figure that the degree of bending of the sensitive material in example 1 is more rounded.
The sensitive materials of example 1 and comparative example 1 were each cured at 72℃for 2 hours to form a disc of 20mm diameter and 3mm thickness, and the degree of deformation was measured by a twin roll machine. The roll gap of the twin-roll machine was set to 1mm, the wafer was set in, and the thickness and recovery time after extrusion thereof were tested.
The discs were placed in a twin roll machine as shown in fig. 22. Deformation is caused during extrusion, and recovery is caused after extrusion. Putting the wafer into a pair roller machine, respectively extruding for 1min, 5min, 10min, 30min and 1h, and taking out. When the extrusion time was 1 to 30 minutes, there was no significant change in the disc after extrusion, and when the extrusion time was 1 hour, the thickness of the disc prepared from the sensitive material in comparative example 1 was changed from 3mm to 2.91mm, and after 30 seconds, was restored to 3mm, whereas the disc prepared from the sensitive material in example 1 was not significantly changed.
And respectively extruding the two wafers in a pair roller for 5s in a way that 1/4 area of each wafer is taken. The sector obtained from the sensitive material in example 1 was cracked at 15 th extrusion and the sector obtained from the sensitive material in comparative example 1 was cracked at 6 th extrusion.
Example 2
A flexible high density scalp electroencephalogram electrode substantially identical to example 1 except that: the carbon conductive material is a single-walled carbon nanotube.
The collected open-close eye signals are processed and mapped, the signal correlation degree of each antenna of the flexible high-density scalp electroencephalogram electrode and the conventional wet electrode-Ag/AgCl electrode is shown in figure 16, the signal-to-noise ratio is shown in figure 17, and the spectrogram is shown in figure 18.
The foregoing has described exemplary embodiments of the invention, it being understood that any simple variations, modifications, or other equivalent arrangements which would not unduly obscure the invention may be made by those skilled in the art without departing from the spirit of the invention.
Claims (10)
1. A flexible high density scalp electroencephalogram electrode, comprising: a carrier and N tantalum filaments, the carrier comprising: the device comprises a substrate and N claw posts connected to the bottom surface of the substrate, wherein each claw post penetrates through one tantalum wire, the bottom end of each tantalum wire is flush with the bottom surface of each claw post and used for collecting ions to form micro-current, the top end of each tantalum wire is located above the substrate and used for being connected with an electrode wire, the carrier is formed by solidifying a sensitive material, and the method for preparing the sensitive material comprises the following steps: uniformly mixing PDMS and an aqueous solution of tetrachloroauric acid, keeping the temperature at 70-80 ℃ for 1-1.5 h, reducing the tetrachloroauric acid into gold particles or gold trichloride, cooling to room temperature, adding a hybrid, and performing ultrasonic treatment to obtain a sensitive material, wherein the hybrid is a mixture of a carbon conductive material and titanium dioxide nano powder, and the mass ratio of the tetrachloroauric acid, the carbon conductive material, the titanium dioxide nano powder and the PDMS in the aqueous solution of tetrachloroauric acid is (0.000003-0.000006): (0.5-3): (0.5-2.5): (92-99) according to the mass parts.
2. The flexible high-density scalp electroencephalogram electrode according to claim 1, wherein the PDMS is formed by mixing a silicone elastomer substrate and a silicone elastomer curing agent, and the ratio of the silicone elastomer substrate to the silicone elastomer curing agent is (9-11): 1 in parts by mass.
3. The flexible high density scalp electroencephalogram electrode according to claim 1 wherein the carbon conductive material is a multi-walled carbon nanotube or a single-walled carbon nanotube.
4. The flexible high density scalp electroencephalogram electrode according to claim 1 wherein the concentration of tetrachloroauric acid in the aqueous solution of tetrachloroauric acid is 10 -6 ～10 -4 mol/L。
5. The flexible high-density scalp electroencephalogram electrode according to claim 1, wherein the length of the tantalum wire is 5-6 cm, the diameter of the tantalum wire is 0.2-0.6 mm, the claw posts are truncated cones tapering from top to bottom, the height of the claw posts is 3-6 mm, the diameter of the bottom surface circle of the claw posts is 1-1.5 mm, the diameter of the top surface circle of the claw posts is 2-2.5 mm, the axial distance between adjacent claw posts is 2.5-4 mm, the base is cylindrical, the diameter of the base is 15-20 mm, and the height of the base is 6-10 mm.
6. A method of preparing a flexible high density scalp electroencephalogram electrode as claimed in claim 1 comprising the steps of:
1) Pouring the sensitive material into a mold twice, and vacuumizing for 10-15 min after each pouring;
2) Inserting N tantalum wires into the sensitive material, keeping the temperature at 60-80 ℃ for 2-5 hours to solidify the sensitive material to form the carrier, and taking out the flexible high-density scalp electroencephalogram electrode from the die.
7. The method according to claim 6, wherein in the step 1), the vacuum is applied to a pressure of-0.08 MPa or less.
8. The method according to claim 7, wherein in the step 1), the mass ratio of the sensitive materials poured into the mold in two steps is (2-3): 5.
9. The conductive liquid is characterized by being formed by mixing sodium carboxymethylcellulose and saturated saline, wherein the ratio of the mass parts of the sodium carboxymethylcellulose to the volume parts of the saturated saline is (1-1.1): 20, the mass parts are in g, and the volume parts are in mL.
10. The conductive fluid of claim 9, wherein the conductive fluid is used in combination with the flexible high density scalp electroencephalogram electrode of claim 1.
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