CN100551462C - Preparation method based on the biological microelectrode array of flexible substrates - Google Patents
Preparation method based on the biological microelectrode array of flexible substrates Download PDFInfo
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- CN100551462C CN100551462C CNB2007100474008A CN200710047400A CN100551462C CN 100551462 C CN100551462 C CN 100551462C CN B2007100474008 A CNB2007100474008 A CN B2007100474008A CN 200710047400 A CN200710047400 A CN 200710047400A CN 100551462 C CN100551462 C CN 100551462C
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- polyimides
- polydimethylsiloxane
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Abstract
The present invention relates to a kind of preparation method of the biological microelectrode array based on flexible substrates, adopt secondary photoetching and electroforming process, apply polydimethylsiloxane sacrifice layer and polyimide acid successively at substrate surface, heat cure forms the polyimides flexible substrates, on flexible substrates by sputter, photoetching and electroforming process prepare metallic circuit, etching metal counterdie then, coating polyimide acid, photoetching and etching polyimide acid, the electroforming metal electrode, heat cure forms polyimides, and the biological microelectrode array based on the polyimides flexible substrates for preparing is stripped down from polydimethylsiloxane.Electrode is positioned at the two ends of metallic circuit, and according to the application requirements electrod-array of arranging, and one at electrode links to each other with biological tissue, and the other end links to each other with stimulator or gauge, and the metallic circuit of electrode bottom links to each other the both sides electrode.The biological microelectrode array of manufacturing of the present invention has the yield rate height, and electrode position is controlled, and impedance is little, advantages such as bio-compatible.
Description
Technical field
The present invention relates to a kind of preparation method of the biological microelectrode array based on flexible substrates, the biological microelectrode array of preparation is used for artificial retina, brain stimulation and measurement electrode etc., belongs to biomedical engineering field.
Background technology
The implantating biological electrode is mainly used in the stimulation of brain and the measurement of brain current, can be applicable to epilepsy or Parkinsonian treatment, also can be applicable in artificial cochlea or the artificial retina, make the blind person see image, the deaf person hears sound, the bioelectrode Development of Preparation Technology will be improved people's living standard greatly.Bioelectrode requires flexible, bio-compatible, and impedance is little, and electrode can be arranged as required.A.Hung is at Microtechnologies in Medicine﹠amp; Introduced a kind of flexible substrates biological microelectrode array preparation method among the Biology 2nd Annual InternationalIEEE-EMB Special Topic Conference on 2-4May 2002:76-79, this method adopts double-deck polyimides technology, electrode adopts the electroforming process preparation, but the biological microelectrode array not insulation each other with this method preparation in use can be short-circuited.N.MacCarthy is at Sensors and Actuators A, 2006, adopt laser that the flexible substrates biological microelectrode array is discharged from substrate among the 132:296-301, microelectrode array with this prepared does not carry out the electroforming second time, its electrode is lower than encapsulation plane 8 μ m, impedance is bigger, needs bigger stimulating current, and discharging microelectrode array needs light-sensitive polyimide and laser equipment.D.C.Rodger is at Nano/Micro Engineered and Molecular System, 2006.NEMS adopt photoresist among the 06.1st IEEEInternational Conference on Jan.2006:743-746 as sacrifice layer, go up preparation flexible substrates biological microelectrode array at Parylene (parylene), microelectrode array with this prepared does not carry out the electroforming second time, its electrode is lower than the encapsulation plane, impedance is bigger, needs bigger stimulating current.For release based on the device of flexible substrate polyimides, people such as Tayfun Akin are at Transactions on biomedical engineering, 1999, reported among the 46:471-480 that employing Ti is as sacrifice layer, with the deionized water corrosion sacrifice layer of 20%HF and 80%, discharge device at last; People such as Xiao Suyan are in " optical precision engineering ", and 2005, then adopt SiO among the 13:674-680
2As sacrifice layer, before discharging at device surface spin coating one deck photoresist with protection Pt resistance and Au electrode, adopting volume ratio then is that 1: 1 HF (49%) and HCl (36%) mixed liquor corrodes sacrifice layer.Adopt metal or SiO
2Make sacrifice layer, there is toxicity in used corrosive liquid, and is unfavorable for the biocompatibility of device.
Utilize microelectromechanical systems (MEMS, Micro Electro Mechanical Systems) processing technique to prepare the main trend that the biologic electrode array with good biocompatibility and electrical parameter becomes biomedical engineering.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of the biological microelectrode array based on flexible substrates is provided, it is simple to have technology, the yield rate height, and electrode position can be arranged as required, and impedance is little, advantages such as bio-compatible.
For realizing this purpose, the present invention adopts secondary photoetching and electroforming process, apply polydimethylsiloxane (PDMS:Polydimethylsiloxane) sacrifice layer and polyimide acid successively at glass or silicon chip substrate surface, heat cure forms the polyimides flexible substrates, on flexible substrates by sputter, photoetching and electroforming process prepare metallic circuit, etching metal counterdie then, coating polyimide acid, photoetching and etching polyimide acid, the electroforming metal electrode, electrode is positioned at the two ends of metallic circuit, and according to the application requirements electrod-array of arranging, one at electrode links to each other with biological tissue, the other end links to each other with stimulator or gauge, the metallic circuit of electrode bottom links to each other the both sides electrode, and last heat cure polyimides strips down the biological microelectrode array based on the polyimides flexible substrates for preparing from polydimethylsiloxane.
Method of the present invention realizes as follows:
1, adopting glass or silicon chip is substrate, uses the washed with de-ionized water substrate, oven dry; Apply 100-500 μ m sacrifice layer polydimethylsiloxane at substrate surface then, apply the thick polyimide acid of 20-100 μ m again on polydimethylsiloxane, heat cure forms the polyimides flexible substrates.
2, at the Cr/Cu metal counterdie of flexible substrates polyimide surface sputter 50-150nm, photoetching then, electroforming gold or copper prepare the highly metallic circuit of 1-10 μ m, live width 5-100 μ m.
3, remove photoresist, remove the Cr/Cu metal counterdie of bottom, apply the thick polyimide acid of 1-5 μ m, photoetching then, etching polyimide acid, electroforming gold, last heat cure forms the polyimides tunic, prepares the biologic electrode array of height 1-5 μ m, diameter 5-200 μ m.
The biological microelectrode array based on flexible substrates that 4, will prepare strips down from polydimethylsiloxane.
The biological microelectrode array advantage based on flexible substrates of utilizing the present invention to make is: (1) technology is simple, and the yield rate height only adopts secondary photoetching electroforming process; (2) electrode position is controlled, can be according to the application requirements electrod-array of arranging; (3) this preparation method adopts the method for encapsulation earlier, back electroforming, and electrode height is higher than the encapsulation plane, has less impedance; (4) adopt biocompatible materials such as polyimides and gold, platinum, good biocompatibility.
Description of drawings
Fig. 1 is the biological microelectrode array structural representation based on flexible substrates provided by the invention.
Among Fig. 1,3 is polyimides (PI), and 4 is the metal counterdie, and 5 is metallic circuit, and 6 is electrode.
Fig. 2 is the biological microelectrode array processing technology flow process based on flexible substrates of the present invention.
Among Fig. 2,1 is substrate, and 2 is polydimethylsiloxane (PDMS), and 3 is polyimides (PI), and 4 is the metal counterdie, and 5 is metallic circuit, and 6 is electrode.
The specific embodiment
Below in conjunction with accompanying drawing and specific embodiment technical scheme of the present invention is further described.Following examples do not constitute limitation of the invention.
Biological microelectrode array structure based on flexible substrates provided by the invention as shown in Figure 1, flexible substrates adopts polyimides 3, at polyimide surface splash-proofing sputtering metal counterdie 4, arrange metallic circuit 5 on the metal counterdie 4, electrode 6 is positioned at the two ends of metallic circuit 5, and according to the application requirements electrod-array of arranging.
The technological process of the inventive method as shown in Figure 2, step 1: apply polydimethylsiloxane 2 and polyimide acid on substrate 1 successively, heat cure forms flexible substrates polyimides 3; Step 2: at flexible substrates polyimides 3 surface sputtering metal counterdies 4, photoetching, electroforming metal circuit 5; Step 3: remove photoresist and metal counterdie, coating polyimide acid, photoetching, etching polyimide acid, electroforming metal electrode 6, heat cure forms polyimides; Step 4: the biological microelectrode array for preparing is stripped down from polydimethylsiloxane 2, obtain flexible substrates biological microelectrode array sample.
Embodiment 1
Biological microelectrode array structural parameters: glass substrate, polydimethylsiloxane thickness 100 μ m, polyimides thickness 50 μ m, golden circuit height 2 μ m, gold electrode height 5 μ m.
(1) flexible substrates preparation
Employing thickness is that the sheet glass of 2mm is a substrate 1, at first carries out substrate and handles: clean with acetone, ethanol and deionized water ultrasonic cleaning, oven dry is 3 hours in 180 ℃ of vacuum drying ovens.Spin coating thickness is the thick polydimethylsiloxane 2 of 100 μ m on substrate then, rotating speed is 1000rpm, be cured in following 2 hours at 80 ℃, spin coating thickness is the polyimide acid of 50 μ m then, rotating speed is 1000rpm, is adopting ladder-elevating temperature method (from 80 ℃--120 ℃--180 ℃--280 ℃) heat cure to form flexible substrates polyimides 3.
(2) metallized metal circuit production
At first at the Cr/Cu metal counterdie 4 of flexible substrates polyimides 3 surface sputtering 50nm, the positive glue AZ4620 that spin coating 4 μ m are thick, adopt the German Karl Suss MA6 of company photo-etching machine exposal, time of exposure is 40 seconds, developing time is 40 seconds, the golden circuit 5 of electroforming thickness 2 μ m, width 20-100 μ m, electric current density 4.4mA/cm
2, 6 minutes electroforming time.
(3) metal electrode is made
At 5.5mW/cm
2Exposure machine exposed 5 minutes down, developed 10 minutes in developer solution then, removed photoresist.The Cr/Cu metal counterdie 4 of polyimide surface adopts the method for argon plasma etching to remove etching power 20kW, gas flow 40sccm, etch period 5 minutes.Apply the thick polyimide acid of 5 μ m then, rotating speed is 4000rpm, the thick positive glue AZ4620 of spin coating 5 μ m on polyimide acid, time of exposure is 50 seconds, and developing time is 60 seconds, with developer solution etching polyimide acid, etch period is 5 minutes, remove photoresist with acetone, the thick gold electrode 6 of electroforming 5 μ m then, electric current density 4.4mA/cm
2, the electroforming time is 15 minutes, and employing ladder-elevating temperature method (from 80 ℃--120 ℃--180 ℃--280 ℃) heat cure formation polyimides tunic.
(4) peel off
The biological microelectrode array based on flexible substrates for preparing is stripped down from polydimethylsiloxane.
Embodiment 2
Biological microelectrode array structural parameters: glass substrate, polydimethylsiloxane thickness 300 μ m, polyimides thickness 20 μ m, golden circuit height 1 μ m, gold electrode height 3 μ m.
(1) flexible substrates preparation
Employing thickness is that the sheet glass of 2mm is a substrate 1, at first carries out substrate and handles: clean with acetone, ethanol and deionized water ultrasonic cleaning, oven dry is 3 hours in 180 ℃ of vacuum drying ovens.Spin coating thickness is the thick polydimethylsiloxane 2 of 300 μ m on substrate then, rotating speed is 700rpm, be cured in following 2 hours at 90 ℃, spin coating thickness is the polyimide acid of 20 μ m then, rotating speed is 2000rpm, and employing ladder-elevating temperature method (from 80 ℃--120 ℃--180 ℃--280 ℃) heat cure formation flexible substrates polyimides 3.
(2) metallic circuit is made
At first at the Cr/Cu metal counterdie 4 of flexible substrates polyimides 3 surface sputtering 100nm, the positive glue AZ4620 that spin coating 2 μ m are thick, adopt the German Karl Suss MA6 of company photo-etching machine exposal, time of exposure is 30 seconds, developing time is 30 seconds, the golden circuit 5 of electroforming thickness 1 μ m, width 20-100 μ m, electric current density 4.4mA/cm
2, 3 minutes electroforming time.
(3) metal electrode is made
At 5.5mW/cm
2Exposure machine exposed 5 minutes down, developed 10 minutes in developer solution then, removed photoresist.The Cr/Cu metal counterdie 4 of polyimide surface adopts the method for argon plasma etching to remove etching power 20kW, gas flow 40sccm, etch period 10 minutes.Apply the thick polyimide acid of 3 μ m then, rotating speed is 4500rpm, the thick positive glue of spin coating 4 μ m on polyimide acid, time of exposure is 50 seconds, and developing time is 40 seconds, with developer solution etching polyimide acid, etch period 3 minutes, remove photoresist with acetone, the thick gold electrode 6 of electroforming 3 μ m then, electric current density 4.4mA/cm
2, the electroforming time is 9 minutes.Employing ladder-elevating temperature method (from 80 ℃--120 ℃--180 ℃--280 ℃) heat cure formation polyimides tunic.
(4) peel off
The biological microelectrode array based on flexible substrates for preparing is stripped down from polydimethylsiloxane.
Biological microelectrode array structural parameters: glass substrate, polydimethylsiloxane thickness 500 μ m, polyimides thickness 100 μ m, copper circuit height 10 μ m, gold electrode height 1 μ m.
(1) flexible substrates preparation
Employing thickness is that the sheet glass of 2mm is a substrate 1, at first carries out substrate and handles: clean with acetone, ethanol and deionized water ultrasonic cleaning, oven dry is 3 hours in 180 ℃ of vacuum drying ovens.Spin coating thickness is the thick polydimethylsiloxane 2 of 500 μ m on substrate then, rotating speed is 500rpm, be cured in following 3 hours at 90 ℃, spin coating thickness is the polyimide acid of 100 μ m then, rotating speed is 500rpm, and employing ladder-elevating temperature method (from 80 ℃--120 ℃--180 ℃--280 ℃) heat cure formation flexible substrates polyimides 3.
(2) metallic circuit is made
At first at the Cr/Cu metal counterdie 4 of flexible substrates polyimides 3 surface sputtering 150nm, the positive glue AZ4620 that spin coating 12 μ m are thick, adopt the German Karl Suss MA6 of company photo-etching machine exposal, time of exposure is 120 seconds, developing time is 120 seconds, the copper circuit 5 of electroforming thickness 10 μ m, width 20-100 μ m, electric current density 4.4mA/cm
2, 30 minutes electroforming time.
(3) metal electrode is made
At 5.5mW/cm
2Exposure machine exposed 5 minutes down, developed 10 minutes in developer solution then, removed photoresist.The Cr/Cu metal counterdie 4 of polyimide surface adopts the method for argon plasma etching to remove etching power 20kW, gas flow 40sccm, etch period 15 minutes.Apply the thick polyimide acid of 1 μ m then, rotating speed is 6000rpm, the thick positive glue of spin coating 2 μ m on polyimide acid, time of exposure is 30 seconds, and developing time is 40 seconds, with developer solution etching polyimide acid, etch period is 1 minute, remove photoresist with acetone, the thick gold electrode 6 of electroforming 1 μ m then, electric current density 4.4mA/cm
2, the electroforming time is 3 minutes.Adopting ladder-elevating temperature method (--120 ℃--180 ℃-280 ℃) heat cure to form the polyimides tunic from 80 ℃.
(4) peel off
The biological microelectrode array based on flexible substrates for preparing is stripped down from polydimethylsiloxane.
Claims (1)
1, a kind of preparation method of the biological microelectrode array based on flexible substrates is characterized in that comprising the steps:
1) adopting glass or silicon chip is substrate, uses the washed with de-ionized water substrate, oven dry; Apply the thick sacrifice layer polydimethylsiloxane of 100-500 μ m at substrate surface then, apply the thick polyimide acid of 20-100 μ m again on polydimethylsiloxane, heat cure forms the polyimides flexible substrates;
2) at the Cr/Cu metal counterdie of polyimides flexible substrates surface sputtering 50-150nm, photoetching then, electroforming gold or copper, the metallic circuit of preparation height 1-10 μ m, live width 5-100 μ m;
3) remove photoresist, remove the Cr/Cu metal counterdie of bottom, apply the thick polyimide acid of 1-5 μ m, photoetching then, the etching polyimide acid, the electroforming gold, last heat cure forms the polyimides tunic, prepares the array of the biological microelectrode of the height 1-5 μ m, the diameter 5-200 μ m that are positioned at the metallic circuit two ends;
The array based on the biological microelectrode of polyimides flexible substrates that 4) will prepare strips down from polydimethylsiloxane.
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