CN102336386B - Three-dimensional solid needle tip flexible micro-electrode array and making method thereof - Google Patents
Three-dimensional solid needle tip flexible micro-electrode array and making method thereof Download PDFInfo
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Abstract
The invention provides a three-dimensional solid needle tip flexible micro-electrode array and a making method thereof. The micro-electrode array comprises a split insulating column array wrapped in an insulating flexible substrate, an electrode and an electricity conducting lead, wherein the head of an insulating column is in a shape of a needle tip and wrapped by the electrode, the needle tip electrode is exposed outside, the electricity conducting lead is paved along the insulating column and the insulating flexible substrate, one end of the electricity conducting lead is connected with the electrode, and the other end is exposed outside. The insulating column is of a solid structure, so that the electrode can be pierced into a stimulation part and effectively provide electric stimulation and record. In order to make the three-dimensional solid needle tip flexible micro-electrode array, silicon materials are treated by a silicon dicing-corrosion process for making the three-dimensional solid needle tip flexible micro-electrode array. The three-dimensional solid needle tip flexible micro-electrode array provided by the invention can be used for nerve electric stimulation and record and can be widely used in the fields of nerve disease treatment, nerve rehabilitation, neurobiology basic research and the like.
Description
Technical field
The present invention relates to a kind of three-dimensional solid needle tip flexible micro-electrode array and preparation method thereof, particularly relate to and utilize silicon scribing-corrosion preparation method to make three-dimensional solid needle tip flexible micro-electrode array, belong to micromachining technology field.
Background technology
The mankind continue for more than 30 years to the research of neural interface.Neural interface, refer to the direct connecting path created between human or animal's nerve (or culture of nerve cell) and external equipment, comprise nerve electrode and peripheral processes circuit part, realize the electro photoluminescence to nerve and record, thus reach the electrical activity improving and analyze cortex.Since the mid-90 in 20th century, this type of knowledge obtained from experiment is in significantly increasing.On zooperal practical basis for many years, the early stage neural interface being applied to human body is designed and creates, for recover to damage the sense of hearing, vision and limb motion ability.Be applied to the microelectrode array of nerve electric stimulation and record as the tightst with nerve connections in neural interface, the most direct part of contact, its performance directly affects application and the efficiency of neural interface.How to produce the good microelectrode array of bio-compatibility, electro photoluminescence and record effect be neural interface research in key issue.
In recent years, owing to there is based on the electrod-array of flexible substrate good bio-compatibility and to organizing less infringement, being widely studied and applied in CO2 laser weld built-in type device.But be generally planar electrode array based on this type of flexible substrate, it is representative that the retina wherein developed with the Y.C.Tai of M.S.Humayun and Caltech of USC (California Institute of Technology) repairs chip most.At file " Flexible Parylene-based Microelectrode Technology for Intraocular Retinal Prostheses " in Proceedings of the 1st IEEE International Conference on Nano/Micro Engineered and Molecular Systems January 18-21, 2006, Zhuhai, China (is applied to the flexible micro-electrode technology based on Parylene that intraocular retina is repaired, first Nano/micron engineering and the meeting of molecular system International Year, January 18-21, 2006, Zhuhai, China) in, they are on the parylene substrate that bio-compatibility is good, prepare the plane electrode chip being integrated with ASIC, success is implanted on eyeball retina, realize electro photoluminescence retina and then by optic nerve, signal is passed to visual cortex, form artificial vision.This plane electrode can meet the requirement of bio-compatibility and the function of electrical conduction preferably, and weak point is that electrode effectively can not be adjacent to tissue, and effect of stimulation is influenced, also just due to this, limits the application that this type of plane electrode is applied to other neural interfaces.
In addition, three-dimensional electrode arrays based on rigid substrate is also widely used in nerve stimulation with record, its three-dimensional needlepoint can penetrate tissue effectively, galvanism and record are provided, " Utah " electrod-array (UTAH MEA) of the Richard Normann research and development of such as Univ Utah USA, as document " Neuronal ensemble control of prosthetic devices by a human with tetraplegia " Vol 442|13July 2006, (nerve for quadriplegia patient controls prosthetic device to nature, 442 volume 13 phases, in July, 2006, nature) report, it develops 96 electrode dot-matrix arrays based on silicon substrate, be named as BrainGate, be applied to intrusive mood brain-computer interface, have and successfully implant the case that cortex makes Patients' rights mechanical arm, mechanical arm can be completed by motion intention to control, the tasks such as computer cursor control, the region of the corresponding arm of the motor cortex returned before its implant is arranged in and hand.Take BrainGate as the Cybernetics company of main product, run after fame in US stock market listing with Cybernetics Neurostream Technologies Inc., aim is the development promoting practical mankind's brain-computer interface technology, worldwide sells its product.But due to the relation of rigid substrate, electrode must strictly be in a fixed position, out-of-flatness surface of can not effectively fitting, also easily causes the damage of tissue.Rigid substrate area can not be too large, limits the scale of electrod-array.In addition, silicon needle point, except making support structure, also needs electrical conduction function, and the electrode self-resistance obtained can comparatively metal electric be very big, and antijamming capability dies down.
So constantly someone proposes based on the improvement of flexible substrate and three-dimensional needlepoint.People's invention disclosed patent (China Patent Publication No. CN101172184 such as Shanghai micro-system institute of Chinese Academy of Sciences Li Gang, denomination of invention " a kind of three-dimensional flexible nervus and preparation method ") in propose a kind of three-dimensional flexible nervus and preparation method thereof, this microelectrode utilizes flexible polymer as base material, designed by the annular patterns of metal seed layer, carry out laddering plating, form the electrode site structure with round and smooth three-dimensional protruding features.But round and smooth projection can not make electric field assemble in tip, and the more important thing is and effectively cannot penetrate tissue, be difficult to reach optimal stimulus effect.Grand once (the China Patent Publication No. CN101398614 in an invention disclosed patent of Beijing University Li Zhi, denomination of invention " a kind of preparation method of the three-dimensional needlepoint electrode array based on Parylene Parylene ") propose and utilize silicon 3 D pinpoint array to prepare three-dimensional needlepoint electrode array based on Parylene (Parylene) flexible substrate, this electrod-array is a kind of Parylene-metal level-Parylene three-decker being similar to sandwich structure, can be used for for artificial retina repair retina under implant surgery.But this flexible substrate array is hollow needle point, can not penetrate tissue, be limit this arrayed applications in the main cause of other nerve stimulations and record.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of three-dimensional solid needle tip flexible micro-electrode array, and this microelectrode array is entity pinpoint array, can penetrate stimulation location, effectively provides electro photoluminescence and record.
Another technical problem that will solve of the present invention is to provide a kind of three-dimensional solid needle tip flexible micro-electrode array preparation method, its method can make entity pinpoint array, stimulation location can be penetrated, electro photoluminescence and record are effectively provided, and cost is low, can accomplish that tip height is large, pattern also can control more even by etching process, and yield rate is high.
Technical scheme of the present invention is: a kind of three-dimensional solid needle tip flexible micro-electrode array, comprise: the flexible substrate 1 of insulation, insulated column 2, needle electrode 3, conductive lead wire 4, wherein be wrapped in discrete insulated column 2 array in the flexible substrate 1 of insulation, discrete insulated column 2 insulated column head is tip-like, wrapped up by needle electrode 3, needlepoint electrode is outside exposed, and conductive lead wire 4 is laid along the flexible substrate 1 of insulated column 2 and insulation, one end is connected with needle electrode 3, and one end is outside exposed in addition.
Described insulated column 2 is solid construction.
Flexible substrate 1 material of described insulation is Parylene.
Described insulated column 2 is silicon posts.
Described needle electrode 3 and conductive lead wire 4 are made up of Metal Cr/Au, and Au is on Cr upper strata.
Metal Cr/Au the thickness of described needle electrode (3) and conductive lead wire (4) is: 15nm/150nm.
The described tip height 400um stating needle electrode (3).
Technical scheme of the present invention also has: three-dimensional solid needle tip flexible micro-electrode array preparation method, comprises the following steps:
Step 1: cleaning silicon chip, LPCVD (chemical vapor deposition) SiO
2/ Si
3n
4;
Step 2: first time silicon chip back side photoetching, forms back-etching SiO
2/ Si
3n
4figure;
Step 3: silicon chip back side dry etching SiO
2/ Si
3n
4, form silicon chip back side TMAH etching mask;
Step 4: silicon chip back side TMAH (TMAH) corrodes silicon, forms silicon groove, for corroding the release of rear silicon;
Step 5: second time silicon chip photoetching, silicon slice dual-surface lithography, forms etching SiO at front side of silicon wafer
2/ Si
3n
4figure, form front TMAH etching mask; Back side dry etching Si
3n
4, then wet etching removes back side SiO
2, to make silicon bonding face smooth;
Step 6: do third time photoetching on the glass sheet, splash-proofing sputtering metal Cr/Au, acetone removes photoresist ultrasonic stripping, makes metal connecting line figure;
Step 7: silicon chip back side and glass front aim at anode linkage;
Step 8: with front side of silicon wafer SiO
2/ Si
3n
4for mask, corrosion obtains discrete silicon post array, simultaneously also isotropic etch glass, defines the side direction undercutting groove under metal connecting line and silicon post;
Step 9: at front side of silicon wafer silicon post arranged in arrays metal electrode, metal electrode is connected with the metal connecting line on sheet glass;
Step 10: deposit ground floor Parylene, and graphically etch Parylene, expose needlepoint electrode;
Step 11:HF wet etching glass, releasing structure, because the side direction undercutting groove under metal connecting line and silicon post is filled by Parylene, releases so metal connecting line and silicon post are also wrapped in by Parylene;
Step 12: back side deposit Parylene, obtains the 3D solid needle point microelectrode array of final flexible substrate.
Silicon caustic solution in described step 8, comprises the following steps:
Step 1: front dry etching SiO
2/ Si
3n
4, form scribe line mark, front side of silicon wafer scribing, form silicon post array;
Step 2: with SiO
2/ Si
3n
4for mask, TMAH corrodes silicon post, silicon post sidewall is plane, silicon post inwardly reduces, and top is the salient angle corrosion of band convex corner compensation mask, forms the salient angle be made up of silicon post sidewall plane, in this process, TMAH corrosion, to back side silicon groove, makes the silicon of silicon groove be separated release, obtains discrete silicon post array;
Step 3: continue SiO
2/ Si
3n
4for mask, HNA (mixed liquor of hydrofluoric acid, nitric acid, glacial acetic acid) isotropic etch silicon, makes silicon top form needle point, and mask comes off after formation needle point; Simultaneously also isotropic etch glass, defines the side direction undercutting groove under metal connecting line and silicon post.
Layout metal electrode method in described step 9, comprise the following steps: front splash-proofing sputtering metal Cr/Au, silicon needle point is wrapped up by metal, due to the existence of side direction undercutting groove, metal separation in the metal that silicon needle point, metal connecting line sputter and glass substrate is opened, and completes the graphical of metal.
Of the present invention have an effect to be: adopt above silicon scribing-corrosion to form silicon post array, cost is low, and the silicon pinpoint array height finally obtained is determined by silicon wafer thickness, and can accomplish that tip height is large, pattern also can control more even by etching process.
The graphical of metal is completed as three-dimensional solid needle tip flexible micro-electrode array preparation method.Avoid the metal patternization photoetching of high step, effectively improve yield rate;
Accompanying drawing explanation
Fig. 1 is a kind of three-dimensional solid needle tip flexible micro-electrode array structural representation of the present invention.
Accompanying drawing indicates: 1 is the flexible substrate 1 insulated; 2 is insulated column; 3 is needle electrode 3; 4 is conductive lead wire 4.
Detailed description of the invention
Illustrate below in conjunction with accompanying drawing and detailed description of the invention the present invention is further described.
Fig. 1 shows the 3D solid needle point microelectrode array of the flexible substrate material based on insulation in stereogram mode, comprise discrete insulated column 2, electrode 3, conductive lead wire 4 in the flexible substrate 1 being wrapped in insulation, wherein insulated column 2 head is tip-like, wrapped up by electrode 3, needlepoint electrode 3 is outside exposed, and conductive lead wire 4 is laid along the flexible substrate 1 of insulated column 2 and insulation, and one end is connected with electrode 3, one end is outside exposed in addition, and described insulated column 2 is solid construction.Conductive lead wire 4 is insulated by double-insulated flexible substrate 1 and is protected, and ensure that the reliability of electrode; Electrode 3 place includes the needle point shape head of three-dimensional protruding insulated column 2, and needle point can penetrate tissue, effectively carries out electro photoluminescence and record; The flexible substrate 1 of whole insulation can with flexible Parylene, effectively to fit out-of-flatness surface, electrode 3, conductive lead wire 4 are Cr/Au, little to tissue injury after implantation, the bio-compatibility of all material is well, and Parylene and the Au bio-compatibility of the real contact of its neutralization tissue are excellent, needle point silicon materials are only as mechanical part, not as electrical conductivity component, make electrode self-resistance little, antijamming capability strengthens.
Three-dimensional solid needle tip flexible micro-electrode array preparation method, comprises the following steps:
LPCVD SiO on the thick N of 400um (100) silicon chip
2/ Si
3n
4, 100nm/100nm; First time back side photoetching, back side dry etching SiO
2/ Si
3n
4, as mask, back side TMAH corrodes silicon 30um, forms silicon groove, for the release of silicon after scribing-corrosion;
Second time photoetching, dual surface lithography, front dry etching SiO
2/ Si
3n
4100nm/100nm, forms scribe line mark, also forms front TMAH etching mask simultaneously; Back side dry etching Si
3n
4100nm, then wet etching removes back side SiO
2, to make silicon bonding face smooth;
Do third time photoetching on the glass sheet, wet etching glass 100nm, splash-proofing sputtering metal Cr/Au 15nm, 150nm, acetone removes photoresist ultrasonic stripping, makes metal connecting line figure;
Silicon chip back side and glass front aim at anode linkage, and the groove gap of 30um makes groove silicon not with on bond glass;
Front side of silicon wafer scribing, silicon chip remains 50um and does not scratch, and forms silicon post array;
Take SiO2/Si3N4 as mask, TMAH corrodes silicon post, silicon post sidewall is <110> face, corrosion rate is higher, silicon post inwardly reduces, top is the salient angle corrosion of band convex corner compensation mask, forms the salient angle be made up of <111>, is about 54.7 degree; In this process, TMAH corrosion, to back side silicon groove, makes the silicon of silicon groove be separated release, obtains discrete silicon pinpoint array; Continue SiO
2/ Si
3n
4for mask, HNA isotropic etch silicon, makes silicon top form needle point, tip height 400um, and mask comes off after formation needle point; Simultaneously also isotropic etch glass, defines the side direction undercutting groove under metal connecting line and silicon post;
Front splash-proofing sputtering metal Cr/Au 15nm/150nm, silicon needle point is wrapped up by metal, and due to the existence of side direction undercutting groove, the metal separation in the metal that silicon needle point, metal connecting line sputter and glass substrate is opened, and completes the graphical of metal;
Deposit ground floor Parylene 10um, and graphically etch Parylene, expose needlepoint electrode;
HF wet etching glass, releasing structure, because the side direction undercutting groove under metal connecting line and silicon post is filled by Parylene, releases so metal connecting line and silicon post are also wrapped in by Parylene; Back side deposit Parylene, obtains the 3D solid pinpoint array of final flexible substrate.
Above content is in conjunction with concrete preferred embodiment further description made for the present invention, comprises material and forms of corrosions such as being not limited to Parylene, silicon, Cr/Au, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (8)
1. a three-dimensional solid needle tip flexible micro-electrode array, comprise the flexible substrate (1) of insulation, insulated column (2), needle electrode (3), conductive lead wire (4), it is characterized in that: be wherein wrapped in discrete insulated column (2) array in the flexible substrate (1) of insulation, discrete insulated column (2) insulated column head is tip-like, wrapped up by needle electrode (3), needlepoint electrode is outside exposed, conductive lead wire (4) is laid along the flexible substrate (1) of insulated column (2) and insulation, one end is connected with needle electrode (3), one end is outside exposed in addition, the three-dimensional solid needle tip flexible micro-electrode array of aforementioned structure adopts micro mechanical technology to process, described insulated column (2) is solid construction, described insulated column (2) is silicon post.
2. a kind of three-dimensional solid needle tip flexible micro-electrode array according to claim 1, is characterized in that: flexible substrate (1) material of described insulation is Parylene.
3. according to a kind of three-dimensional solid needle tip flexible micro-electrode array one of claim 1 or 2 Suo Shu, it is characterized in that: described needle electrode (3) and conductive lead wire (4) are made up of Metal Cr/Au, and Au is on Cr upper strata.
4. a kind of three-dimensional solid needle tip flexible micro-electrode array according to claim 3, is characterized in that: the Metal Cr/Au thickness of described needle electrode (3) and conductive lead wire (4) is: 15nm/150nm.
5. a kind of three-dimensional solid needle tip flexible micro-electrode array according to claim 3, is characterized in that: described in state the tip height 400um of needle electrode (3).
6. a three-dimensional solid needle tip flexible micro-electrode array preparation method as claimed in claim 1, is characterized in that, comprise the following steps:
Step 1: cleaning silicon chip, chemical vapor deposition SiO
2/ Si
3n
4;
Step 2: first time silicon chip back side photoetching, forms back-etching SiO
2/ Si
3n
4figure;
Step 3: silicon chip back side dry etching SiO
2/ Si
3n
4, form silicon chip back side TMAH etching mask;
Step 4: silicon chip back side TMAH corrosion silicon, forms silicon groove, for corroding the release of rear silicon;
Step 5: second time silicon chip photoetching, silicon slice dual-surface lithography, forms etching SiO at front side of silicon wafer
2/ Si
3n
4figure, form front TMAH etching mask; Back side dry etching Si
3n
4, then wet etching removes back side SiO
2, to make silicon bonding face smooth;
Step 6: do third time photoetching on the glass sheet, splash-proofing sputtering metal Cr/Au, acetone removes photoresist ultrasonic stripping, makes metal connecting line figure;
Step 7: silicon chip back side and glass front aim at anode linkage;
Step 8: with front side of silicon wafer SiO
2/ Si
3n
4for mask, corrosion obtains discrete silicon post array, simultaneously also isotropic etch glass, defines the side direction undercutting groove under metal connecting line and silicon post;
Step 9: at front side of silicon wafer silicon post arranged in arrays metal electrode, metal electrode is connected with the metal connecting line on sheet glass;
Step 10: deposit ground floor Parylene, and graphically etch Parylene, expose needlepoint electrode;
Step 11:HF wet etching glass, releasing structure, because the side direction undercutting groove under metal connecting line and silicon post is filled by Parylene, releases so metal connecting line and silicon post are also wrapped in by Parylene;
Step 12: back side deposit Parylene, obtains the 3D solid needle point microelectrode array of final flexible substrate.
7. a three-dimensional solid needle tip flexible micro-electrode array preparation method as claimed in claim 6, is characterized in that: the silicon caustic solution in described step 8, comprises the following steps:
Step 1: front dry etching SiO
2/ Si
3n
4, form scribe line mark, front side of silicon wafer scribing, form silicon post array;
Step 2: with SiO
2/ Si
3n
4for mask, TMAH corrodes silicon post, silicon post sidewall is plane, silicon post inwardly reduces, and top is the salient angle corrosion of band convex corner compensation mask, forms the salient angle be made up of silicon post sidewall plane, in this process, TMAH corrosion, to back side silicon groove, makes the silicon of silicon groove be separated release, obtains discrete silicon post array;
Step 3: continue SiO
2/ Si
3n
4for mask, the mixed liquor isotropic etch silicon of hydrofluoric acid, nitric acid, glacial acetic acid, makes silicon top form needle point, and mask comes off after formation needle point; Simultaneously also isotropic etch glass, defines the side direction undercutting groove under metal connecting line and silicon post.
8. a three-dimensional solid needle tip flexible micro-electrode array preparation method as claimed in claims 6 or 7, it is characterized in that: the layout metal electrode method in described step 9, comprise the following steps: front splash-proofing sputtering metal Cr/Au, silicon needle point is wrapped up by metal, due to the existence of side direction undercutting groove, metal separation in the metal that silicon needle point, metal connecting line sputter and glass substrate is opened, and completes the graphical of metal.
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| CN102670193A (en) * | 2012-05-09 | 2012-09-19 | 中国科学院上海技术物理研究所 | Hybrid three-dimensional neuron probe array |
| CN102755691A (en) * | 2012-06-19 | 2012-10-31 | 吉林大学 | Medical high-sensitivity micro needle array electrode |
| CN106865491B (en) * | 2015-12-14 | 2019-07-19 | 国网智能电网研究院 | A kind of nano-electrode array and preparation method thereof |
| CN107224666B (en) * | 2017-05-15 | 2023-03-24 | 杭州暖芯迦电子科技有限公司 | Nerve stimulation electrode and manufacturing method thereof |
| CN208492977U (en) * | 2017-05-19 | 2019-02-15 | 山东大学 | Multilayered structure flexibility artificial hearing Neural stimulation electrodes |
| CN112631425B (en) * | 2020-12-21 | 2022-03-22 | 上海交通大学 | Microneedle array type brain-computer interface device and preparation method thereof |
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| CN101721200A (en) * | 2008-10-10 | 2010-06-09 | 大学共同利用机关法人自然科学研究机构 | Pain sensory nerve stimulation apparatus |
| US7949412B1 (en) * | 2005-06-02 | 2011-05-24 | Advanced Bionics, Llc | Coated electrode array having uncoated electrode contacts |
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| WO2005114720A2 (en) * | 2004-05-14 | 2005-12-01 | California Institute Of Technology | Parylene-based flexible multi-electrode arrays for neuronal stimulation and recording and methods for manufacturing the same |
| DE102005019968A1 (en) * | 2005-04-29 | 2006-11-02 | Valerij Ortmann | Biostable neuroelectrode for deriving electrical signals/electrically stimulating neuronal tissue, comprises flexible and/or rigid substrate from electric conductive/non-conductive material, and electrodes arranged in the substrate surface |
| US8700178B2 (en) * | 2005-12-27 | 2014-04-15 | Boston Scientific Neuromodulation Corporation | Stimulator leads and methods for lead fabrication |
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| US7949412B1 (en) * | 2005-06-02 | 2011-05-24 | Advanced Bionics, Llc | Coated electrode array having uncoated electrode contacts |
| CN101721200A (en) * | 2008-10-10 | 2010-06-09 | 大学共同利用机关法人自然科学研究机构 | Pain sensory nerve stimulation apparatus |
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