CN114271828A - Degradable high-array flexible device for brain-computer interface and preparation method thereof - Google Patents
Degradable high-array flexible device for brain-computer interface and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a degradable high-array flexible device for a brain-computer interface, which comprises a flexible substrate, a flexible conductive electrode, a supporting layer, an electric insulating layer and a semiconductor layer which are sequentially laminated, wherein the flexible conductive electrode, the electric insulating layer and the semiconductor layer jointly form an organic electrochemical transistor array for collecting, amplifying and transmitting weak electroencephalograms. The flexible sensing device is made of materials with good biocompatibility and biodegradability, can perfectly fit a curved topological structure of the brain, realizes a novel cerebral cortex monitoring device with co-fused and full-covered appearance, can be used as a signal recording sensor to amplify weak electroencephalogram signals and remarkably improve the signal-to-noise ratio and the signal acquisition capacity, ensures high-density multiplexing through an organic electrochemical transistor array structure, enables the acquired signals to have higher-level space-time resolution, and can monitor and record physiological electrical signals on a cell level in a breakthrough manner.
Description
Technical Field
The invention relates to the field of flexible electronic technology and artificial intelligence, in particular to a degradable high-array flexible device for electroencephalogram signal monitoring and brain-computer interfaces and an implementation method thereof.
Background
In the foreseeable future, artificial intelligence and machine intelligence are gradually integrated, the storage and operation capabilities of machines are fully exerted, the thinking and innovation capabilities of human brains are fused, and brain-machine intelligence fusion is realized. The brain-computer interface establishes a brand-new communication and control channel independent of peripheral nerves and muscles between the brain and the external environment, so that the direct interaction between the brain and the external equipment is realized. The technology can establish communication between the brain of a human (or other animal) and the external environment to achieve the purpose of controlling equipment, and further play roles in monitoring, replacing, improving/recovering, enhancing and supplementing.
Therefore, the method is very important for monitoring the high sensitivity and the high time-space resolution of the electroencephalogram signals. The physiological electric signal belongs to an unstable weak signal under a strong noise background, and has the characteristics of strong noise, weak signal, low frequency, strong randomness and the like. Traditionally, non-invasive methods have been used to place electrodes on the scalp of the brain to measure the current flow of brain activity. However, scalp electroencephalogram signals are small, interference noise is high, and detection results are easy to distort. Invasive electroencephalogram monitoring requires the implantation of devices into the surface or into the cortex of the brain (epidural or subdural) by neurosurgery. The invasive device can be stably placed for a long time, the electrical activity of the nerve cell is directly recorded, the signal attenuation is small, and the signal-to-noise ratio and the spatial resolution are far higher than those of a non-invasive device. The cortical monitoring electrode needs to be completely implanted, belongs to traumatic implantation, has great technical difficulty and secondary infection possibility, and once craniocerebral infection, electrode failure or electrode life is over, the electrode needs to be taken out, so that secondary injury can be caused. Therefore, the minimally invasive implantation of the cerebral cortex is easier to be put into practical use than the intracortical implantation. In addition, most invasive monitoring electrodes are rigid, such as typically represented by michigan and utah electrodes, have much higher hardness than brain tissue, are difficult to move with the brain, and are prone to callus formation, thereby attenuating signals. Therefore, a novel cerebral cortex monitoring device which is flexible and can realize shape co-fusion and full coverage with the bending topological structure of the brain is bound to become a future development trend.
Different from the in-situ recording of the traditional nerve electrode, the organic electrochemical transistor can further amplify weak cardiac and cerebral electrical signals and obviously improve the signal to noise ratio, and has been deeply researched and applied to the monitoring and recording of physiological electrical signals. Meanwhile, the mechanical characteristics of the ultrathin and soft organic electrochemical transistor allow the organic electrochemical transistor to be closely attached to biological tissues for a long time, the impedance and the sliding of the device and the skin interface are reduced, and the motion artifact is reduced to the maximum extent so as to carry out continuous high-fidelity monitoring. However, in practical applications, the flexible organic electrochemical transistor still lacks of a biodegradable conductive channel material with high sensitivity, and a matched flexible process technology and a multi-channel device structure design, so that the development of a degradable organic electrochemical transistor array is greatly limited. Non-degradable organic electrochemical transistors cause chronic immune reactions in visceral tissues, requiring secondary surgery for device replacement or removal. The OECT arrays reported to date have a low number of samples that do not adequately cover the full picture of brain activity. Thus, improvements are needed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a degradable high-array flexible device for a brain-computer interface and an implementation method thereof, which are combined with material engineering, flexible electronic technology, biomedical engineering and the like and mainly used for solving the problems of weak signal acquisition capacity, low rigidity, low space-time resolution and the like of the traditional nerve electrode.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a degradable high-array flexible device for brain-computer interface comprises
A flexible substrate made of a biodegradable polymer synthesized by an ester bond;
the flexible conductive electrode is made by adopting metal or alloy material with good conductivity, electrochemical stability, biological safety and degradability to be photoetched on the flexible substrate according to the patterning of the organic electrochemical transistor array;
the supporting layer is made by coating biodegradable organic insulating materials on the flexible substrate and the flexible conductive electrode and is used for preventing the flexible substrate from being dissolved by the electric insulating layer;
the electric insulating layer is made by adopting a polymer material with high dielectric constant and good chemical stability and photoetching the support layer according to the patterning of the organic electrochemical transistor array;
the semiconductor layer is made by adopting a biologically safe semiconductor material which has high carrier mobility and large unit body capacitance and can sensitively respond to local potential change and is patterned and photoetched on the electric insulating layer according to an organic electrochemical transistor array;
the organic electrochemical transistor array for collecting, amplifying and transmitting weak electroencephalogram signals is formed by a flexible conductive electrode, an electric insulating layer and a semiconductor layer.
Specifically, the thickness of the flexible substrate is 10-20 μm, the thickness of the flexible conductive electrode is 50-100nm, the thickness of the supporting layer is 0.5-1 μm, the thickness of the electric insulating layer is 1-2 μm, and the thickness of the semiconductor layer is 100-200 nm.
Specifically, the flexible substrate is made of one of polylactic acid-glycolic acid copolymer, polycaprolactone and polyglycolide.
Specifically, the flexible conductive electrode adopts at least one of pure magnesium, magnesium calcium, magnesium strontium, magnesium zinc, magnesium lithium, magnesium tin, magnesium- (silicon, manganese, zirconium and silver), magnesium yttrium, magnesium zinc rare earth, magnesium neodymium zinc-based alloy, magnesium- (gadolinium, lanthanum, cerium and dysprosium), iron-based alloy, zinc-based alloy, bulk amorphous alloy and doped conductive polymer.
Specifically, the support layer adopts polyvinyl alcohol.
Specifically, the electric insulation layer adopts one of sugar natural dielectric or synthetic polymers.
Specifically, the semiconductor layer is made of one of poly (3-hexylthiophene), a donor-acceptor copolymer, and a P3HT derivative mixed with poly (butylene succinate), polylactic acid, poly (ester urea), and a carboxylic ester substituent of polyurethane.
Based on the above structure, the invention also provides a preparation method of the degradable high-array flexible device for the brain-computer interface, which comprises the following steps:
and 7, soaking the treated whole body in deionized water, and peeling the device from the substrate from the edge of the flexible substrate to obtain the degradable high-array flexible device for the brain-computer interface.
Specifically, the process of performing the patterning lithography process in step 3, step 5, and step 6 is as follows:
and (3) spin-coating photoresist on the cooled layer, and then sequentially carrying out exposure, development, plasma etching and photoresist removal to obtain the patterned flexible conductive electrode, the electric insulating layer or the semiconductor layer.
Specifically, the flexible substrate is made of PLGA material, the flexible conductive electrode is made of gold material, the supporting layer is made of PVA material, the electric insulating layer is made of PVA material, and the semiconductor layer is made of PEDOT PSS material.
Compared with the prior art, the invention has the following beneficial effects:
the flexible sensing device based on the organic electrochemical transistor array structure is made of materials with good biocompatibility and biodegradability, can perfectly fit the curved topological structure of the brain, realizes a novel cerebral cortex monitoring device with co-fused and full-covered appearance, can be used as a signal recording sensor to amplify weak electroencephalogram signals and remarkably improve the signal-to-noise ratio and the signal acquisition capacity, ensures high-density multiplexing through the organic electrochemical transistor array structure, enables the acquired signals to have higher-level space-time resolution, can monitor and record physiological electrical signals on a cell level in a breakthrough manner, and effectively avoids the problems of infection, trauma, operation cost and the like caused by secondary operations in practical application due to the good biological characteristics of the materials. Is suitable for application in electroencephalogram signal monitoring.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
Fig. 2 is a schematic structural diagram of array integration in an embodiment of the present invention.
FIG. 3 is a graph of experimental data for example 1 of the present invention, in which FIG. 3(a) is an output characteristic curve of a single device, FIG. 3(b) is a transfer characteristic curve, FIG. 3(c) is a graph of a 5Hz AC signal trace, and FIG. 3(d) is a graph of yield degradation of an array of 100 cells.
Fig. 4 is a graph showing experimental data of example 2 of the present invention, in which fig. 4(a) is an output characteristic curve of a single device, fig. 4(b) is a transfer characteristic curve, fig. 4(c) is a graph showing a recording of a 50Hz ac signal, and fig. 4(d) is a graph showing a high-temperature accelerated degradation product of the device.
Detailed Description
The present invention is further illustrated by the following figures and examples, which include, but are not limited to, the following examples.
Examples
As shown in fig. 1 to fig. 2, the degradable high-array flexible device for a brain-computer interface mainly includes a flexible substrate 1, a flexible conductive electrode 2, a support layer 3, an electrical insulation layer 4, a semiconductor layer 5, and in practical application, may further include an encapsulation layer. The organic electrochemical transistor array for collecting, amplifying and transmitting weak electroencephalogram signals is formed by a flexible conductive electrode, an electric insulating layer and a semiconductor layer.
The flexible substrate is 10-20 microns thick, is made of a biodegradable polymer synthesized by an ester bond, such as polylactic acid, polycaprolactone, polyglycolide and the like, and can realize active degradation through hydrolysis reaction. Similarly, other chemically and enzymatically hydrolytically degradable moieties include amide, thioester, anhydride, carbonate, urea, carbamate, imide, and imine linkages, etc., which serve as sites on the polymer backbone for decomposition under biologically benign conditions. Polylactic-co-glycolic acid (PLGA) is preferably used as the substrate in the embodiment, and is flexible and degradable.
The flexible conductive electrode is 50-100nm thick, and is made of metal or alloy materials with good conductivity, electrochemical stability, biological safety and degradability, such as one or more combinations of degradable metal systems of pure magnesium, magnesium calcium, magnesium strontium, magnesium zinc, magnesium lithium, magnesium tin, magnesium- (silicon, manganese, zirconium, silver), magnesium yttrium, magnesium zinc rare earth, magnesium neodymium zinc-based alloy, magnesium- (gadolinium, lanthanum, cerium, dysprosium), iron-based alloy, zinc-based alloy, bulk amorphous alloy and the like, or doped conductive polymers, such as polypyrrole, polyaniline, poly (3, 4-ethylenedioxythiophene) and the like, wherein the conductivity of the doped conductive polymers is generally lower than that of the metal electrode. In this embodiment, a gold (Au) electrode is deposited on a flexible substrate by evaporation, and then a patterned flexible conductive electrode is formed by photolithography.
The thickness of the supporting layer is 0.5-1 μm, and the supporting layer is made of biodegradable organic insulating material and is determined according to the solvent characteristics of the substrate and the electric insulating layer, and is mainly used for preventing the electric insulating layer from dissolving the substrate. Polyvinyl alcohol (PVA) is preferred as the support layer in the present invention.
The thickness of the electric insulating layer is 1-2 μm, the electric insulating layer adopts polymer materials with high dielectric constant and good chemical stability, such as sugar natural dielectrics, e.g. glucose, lactose and the like, the dielectric constant at 1kHz is 6.35 and 6.55 respectively, and the breakdown voltage is 1.5MV/cm and 4.5MV/cm respectively. The saccharides can effectively prepare a sealing film without pores by using water or dimethyl sulfoxide as a solvent. Meanwhile, synthetic polymers such as poly (glycerol sebacate) can also be used as highly efficient degradable dielectric materials. In this embodiment, the electrical insulating layer is preferably a poly (lactic-co-glycolic acid) that is spin coated on the support layer and then photolithographically processed to form a patterned electrical insulating layer.
The thickness of the semiconductor layer is 100-200nm, and the semiconductor material is a biologically safe semiconductor material which has high carrier mobility and large unit volume capacitance and can sensitively respond to local potential change, such as poly (3-hexylthiophene, P3HT), donor-acceptor copolymer (for example, diketopyrrolopyrrole) or P3HT derivative of carboxylate substituent, and after poly (butylene succinate), polylactic acid, poly (ester urea) and polyurethane are mixed in proper proportion, the semiconductor material not only has the electrical property and mechanical flexibility of a semiconductor, but also has biodegradability. The semiconductor material in this embodiment is preferably poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid (PEDOT: PSS).
Based on the above construction and materials, the preparation method of the degradable high-array flexible device for the brain-computer interface comprises the following steps:
and 7, soaking the treated whole body in deionized water for 1 hour, and peeling the device from the substrate from the edge of the flexible substrate to obtain the degradable high-array flexible device for the brain-computer interface.
Example 1
This embodiment provides a specific degradable high array flexible Device, which may be referred to as Device 1(Device 1), and its structure is from bottom to top in order:
PLGA(12μm)/Au(100nm)/PVA(500nm)/PLGA(1.5μm)/PEDOT:PSS(150nm)
the preparation method comprises the following steps:
step 1: cleaning the glass substrate by using a detergent, deionized water, acetone and isopropanol, and then drying;
step 2: spin-coating a degradable base material PLGA (20 wt.% dissolved in chloroform) on the dried glass substrate, and then carrying out annealing treatment;
and step 3: and putting the cooled substrate into a vacuum evaporation chamber, and evaporating and plating a layer of Au on the substrate to be used as a conductive electrode. After cooling, spin-coating AZ5214 photoresist, and then sequentially carrying out exposure, development, wet etching and photoresist removal to obtain a patterned Au electrode;
and 4, step 4: PVA (4 wt.%, dissolved in water) was spin-coated on the Au electrode, followed by annealing;
and 5: a dot insulating layer PVA (5 wt.%, dissolved in chloroform) was spin-coated on the PVA, and then subjected to an annealing treatment. After cooling, spin-coating AZ5214 photoresist, and then sequentially carrying out exposure, development, plasma etching and photoresist removal to obtain patterned PVA/PLGA;
step 6: based on the above step, a mixed solvent of PEDOT: PSS (2mL of 3, 4-ethylenedioxythiophene, 0.5 wt.% ethylene glycol, 0.01 wt.% dodecylbenzenesulfonic acid, 0.1 wt.% 3- (2, 3-glycidoxy) propyltrimethoxysilane) was spin-coated as a semiconductor layer, followed by annealing for 1 hour. And after cooling, spin-coating AZ5214 photoresist, and then sequentially carrying out exposure, development, plasma etching and photoresist removal to obtain the patterned PEDOT: PSS.
And 7: and soaking the device in deionized water for 1 hour, and stripping from the edge to obtain the complete device.
The obtained device 1 was tested, and the test results are shown in fig. 3(a) to (d).
Example 2
This embodiment provides a specific degradable high array flexible Device, which may be referred to as Device 2(Device 2), and its structure is from bottom to top in order:
PLGA(12μm)/Au(100nm)/PVA(500nm)/PLGA(1.5μm)/gDpp-g2T(150nm)
the preparation method comprises the following steps:
step 1: cleaning the glass substrate by using a detergent, deionized water, acetone and isopropanol, and then drying;
step 2: spin-coating a degradable base material PLGA (20 wt.% dissolved in chloroform) on the dried glass substrate, and then carrying out annealing treatment;
and step 3: and putting the cooled substrate into a vacuum evaporation chamber, and evaporating and plating a layer of Au on the substrate to be used as a conductive electrode. After cooling, spin-coating AZ5214 photoresist, and then sequentially carrying out exposure, development, wet etching and photoresist removal to obtain a patterned Au electrode;
and 4, step 4: PVA (4 wt.%, dissolved in water) was spin-coated on the Au electrode, followed by annealing;
and 5: a dot insulating layer PVA (5 wt.%, dissolved in chloroform) was spin-coated on the PVA, and then subjected to an annealing treatment.
Step 6: spin-coating PVA (4 wt.% dissolved in water) on an Au electrode, then carrying out annealing treatment, cooling, then spin-coating AZ5214 photoresist, and then sequentially carrying out exposure, development, plasma etching and photoresist removal to obtain patterned PVA/PLGA/PVA;
and 7: gDpp-g2T (8mg/ml, dissolved in chloroform) was spin-coated as a semiconductor layer on the basis of the above step, followed by annealing for 1 hour. And after cooling, spin-coating AZ5214 photoresist, and then sequentially carrying out exposure, development, plasma etching and photoresist removal to obtain the patterned gDpp-g 2T.
And 8: and soaking the device in deionized water for 1 hour, and stripping from the edge to obtain the complete device.
The obtained device 2 was tested, and the test results are shown in fig. 4(a) to (d).
According to the test results, the degradable high-array flexible device prepared by the invention has excellent performance and is suitable for being applied to electroencephalogram signal monitoring.
The above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, but all changes that can be made by applying the principles of the present invention and performing non-inventive work on the basis of the principles shall fall within the scope of the present invention.
Claims (10)
1. A degradable high-array flexible device for a brain-computer interface is characterized by comprising
A flexible substrate made of a biodegradable polymer synthesized by an ester bond;
the flexible conductive electrode is made by adopting metal or alloy material with good conductivity, electrochemical stability, biological safety and degradability to be photoetched on the flexible substrate according to the patterning of the organic electrochemical transistor array;
the supporting layer is made by coating biodegradable organic insulating materials on the flexible substrate and the flexible conductive electrode and is used for preventing the flexible substrate from being dissolved by the electric insulating layer;
the electric insulating layer is made by adopting a polymer material with high dielectric constant and good chemical stability and photoetching the support layer according to the patterning of the organic electrochemical transistor array;
the semiconductor layer is made by adopting a biologically safe semiconductor material which has high carrier mobility and large unit body capacitance and can sensitively respond to local potential change and is patterned and photoetched on the electric insulating layer according to an organic electrochemical transistor array;
the organic electrochemical transistor array for collecting, amplifying and transmitting weak electroencephalogram signals is formed by a flexible conductive electrode, an electric insulating layer and a semiconductor layer.
2. The degradable high-array flexible device for the brain-computer interface as claimed in claim 1, wherein the thickness of the flexible substrate is 10-20 μm, the thickness of the flexible conductive electrode is 50-100nm, the thickness of the support layer is 0.5-1 μm, the thickness of the electrical insulation layer is 1-2 μm, and the thickness of the semiconductor layer is 100-200 nm.
3. The degradable high-array flexible device for a brain-computer interface of claim 1, wherein the flexible substrate is made of one of poly (lactic-co-glycolic acid), polycaprolactone, and polyglycolide.
4. The degradable high array flexible device for a brain-computer interface of claim 1, wherein the flexible conductive electrode employs at least one of pure magnesium, magnesium calcium, magnesium strontium, magnesium zinc, magnesium lithium, magnesium tin, magnesium- (silicon, manganese, zirconium, silver), magnesium yttrium, magnesium zinc rare earth, magnesium neodymium zinc base alloy, magnesium- (gadolinium, lanthanum, cerium, dysprosium), iron base alloy, zinc base alloy, bulk amorphous alloy, doped conductive polymer.
5. The degradable high-array flexible device for a brain-computer interface of claim 1, wherein the support layer is polyvinyl alcohol.
6. The degradable high array flexible device for a brain-computer interface of claim 1, wherein the electrically insulating layer is one of a sugar based natural dielectric or a synthetic polymer.
7. The degradable high-array flexible device for brain-computer interface of claim 1, wherein said semiconductor layer is one of poly (3-hexylthiophene), donor-acceptor copolymer, P3HT derivative mixed with carboxylic ester substituent of poly (butylene succinate), polylactic acid, poly (ester urea), polyurethane.
8. The method for preparing the degradable high-array flexible device for the brain-computer interface according to any one of claims 1 to 7, comprising the following steps:
step 1, drying the cleaned substrate;
step 2, spin-coating a biodegradable polymer material on the dried substrate, and then carrying out annealing treatment to obtain a substrate with a flexible substrate;
step 3, putting the substrate with the flexible substrate into a vacuum evaporation chamber, evaporating a conductive electrode layer on the flexible substrate, cooling, and carrying out patterned photoetching treatment on the conductive electrode layer according to the organic electrochemical transistor array to form a flexible conductive electrode on the flexible substrate;
step 4, spin-coating an organic insulating material on the patterned flexible conductive electrode and the corresponding flexible substrate, and then carrying out annealing treatment to form a supporting layer;
step 5, spin-coating a polymer material with high dielectric constant and good chemical stability on the supporting layer to form an electric insulating layer, carrying out patterned photoetching treatment on the electric insulating layer according to the organic electrochemical transistor array after annealing treatment and cooling, and forming a patterned electric insulating layer on the supporting layer;
step 6, spin-coating a semiconductor material on the patterned electric insulating layer and the corresponding supporting layer to form a semiconductor layer, and carrying out patterned photoetching treatment on the semiconductor layer according to the organic electrochemical transistor array after annealing treatment and cooling to form a patterned semiconductor layer;
and 7, soaking the treated whole body in deionized water, and peeling the device from the substrate from the edge of the flexible substrate to obtain the degradable high-array flexible device for the brain-computer interface.
9. The method for manufacturing the degradable high-array flexible device for the brain-computer interface according to claim 8, wherein the patterning lithography process in the steps 3, 5 and 6 is as follows:
and (3) spin-coating photoresist on the cooled layer, and then sequentially carrying out exposure, development, plasma etching and photoresist removal to obtain the patterned flexible conductive electrode, the electric insulating layer or the semiconductor layer.
10. The method for preparing the degradable high-array flexible device for the brain-computer interface of claim 8, wherein the flexible substrate is made of PLGA material, the flexible conductive electrode is made of gold material, the support layer is made of PVA material, the electric insulation layer is made of PVA material, and the semiconductor layer is made of PEDOT PSS material.
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