CN102817057B - Graphene oxide/conducting polymer composite deposite and preparation method thereof - Google Patents
Graphene oxide/conducting polymer composite deposite and preparation method thereof Download PDFInfo
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Abstract
Disclosure one graphene oxide/conducting polymer composite deposite and preparation method thereof, including: first weigh graphene oxide and conducting polymer monomer adds in scrubbing water, utilize ultrasonic and stirring to be made into electroplating aqueous solution, in aqueous solution, be blown into nitrogen discharge oxygen in solution；Then by needing the electrode of plating and in electrode immersion plating solution, connecing positive source and negative pole respectively, electroplating through after a while is needing the coating that on electroplated electrode, formation graphene oxide and conducting polymer uniformly mix.Graphene oxide prepared by the present invention/conducting polymer composite deposite stable homogeneous, the electric property having had, stability and biocompatibility, it is possible to be used to make implantating biological armarium.
Description
Technical field
The present invention relates to the composite deposite in a kind of biomedical engineering technology field and preparation method thereof, specifically graphene oxide/conducting polymer composite deposite and preparation method thereof.
Background technology
Use implantating biological microelectrode can implement functional electrical stimulation or physiology electric record.As electricity device and biological tissue's interface, electrode points decorative material is the key factor determining biological microelectrode performance.Can safely and effectively working for guaranteeing that biological microelectrode is implanted in live body, electrode points decorative material should have excellent following properties: chemical property, i.e. Low ESR and big electric charge injection capacity；Stability, namely through repeatedly using the chemical property still keeping excellent；Biocompatibility, will not cause biological rejection or tissue necrosis after namely implanting.
Conducting polymer has many-sided excellent characteristic, for instance can be adulterated by difference and be conveniently carried out the electrochemical properties of varied modified, good biocompatibility and excellence, thus being widely used in multiple field in the last few years.Emerging nano material Graphene, constantly shows the excellent performance of each side, and becomes the focus studied now because of it.Utilize graphene oxide as counter ion counterionsl gegenions and the conducting polymer composite deposite by electrochemical synthesis, combine both superior functions, meet the requirements as electrode points decorative material.Its preparation process is simple and cost is low, it is easy to be modified according to different performance demand feed change kind and proportioning.
Find by prior art documents, KipALudwig, NicholasBLanghals etc. write articles " Poly (3; 4-ethylenedioxythiophene) (PEDOT) polymercoatingsfacilitatesmallerneuralrecordingelectrode s " (" poly-(3,4-ethylene dioxythiophene) (PEDOT) polymer coating promotes less neural recording electrode " " neural engineering periodical ") at JOURNALOFNEURALENGINEERING.8 (2011) 014001.The document is referred to preparation and the measuring technology of the nerve electrode that a kind of conducting polymer PEDOT coating is modified.This technology synthesizes PEDOT by constant current process at electrode points surface electrochemistry, improves the electric property of electrode.Its shortcoming is in that to use perchlorate not good as the polymer coating stability of counter ion counterionsl gegenions.After the electricity irritation repeated in a large number in the long period or electrographic recording, coating pattern can change, even cracking or peel off.This can largely effect on the electric property of electrode, and small coating spall likely remains in bodily tissue, has the danger causing health hazard.Therefore, this conducting polymer coating is not suitable for being chronically implanted biologic medical electro physiology equipment for manufacturing.
Summary of the invention
The present invention is directed to prior art above shortcomings, it is provided that a kind of graphene oxide/conducting polymer composite deposite and preparation method thereof.The electric property using the bioelectrode that this composite deposite modifies is greatly improved, and the stability that had of coating and biocompatibility, it is possible to be used to make implantating biological armarium.Its manufacturing process is simple to operation, and utilizes the easily controllable coating shape of electrochemical method for synthesizing, size and performance.Overall cost of manufacture is low, is beneficial to a large amount of preparation.
The present invention is achieved by the following technical solutions:
First weigh graphene oxide and conducting polymer monomer to add in scrubbing water, utilize ultrasonic and stirring to be made into electroplating aqueous solution, in aqueous solution, be blown into nitrogen prevent monomer oxidation；
Then by needing the electrode of plating and in electrode immersion plating solution, connecing positive source and negative pole respectively, electroplating through after a while is needing the coating that on electroplated electrode, formation graphene oxide and conducting polymer uniformly mix.
Described graphene oxide refers to the Graphene with negative charge groups such as carboxyl, hydroxyl, sulfonic group, epoxy radicals, and it has good water dispersible.
Described conducting polymer monomer refers in the derivatives of 3,4-ethylenedioxy thiophene (EDOT), thiophene (Th), pyrroles (Py), aniline (An) and above each monomer a kind of.
Described scrubbing water refers to deionized water or ultra-pure water.
Described ultrasonic refer to that to be placed in ultrasonic cleaner by the mixed solution container filling graphene oxide, conducting polymer monomer and scrubbing water ultrasonic and exceed half an hour, form uniform graphene oxide dispersion.
It is super after an hour that described stirring refers to that rotating speed stirs mixed liquor more than 100 revs/min, forms the electroplating aqueous solution of stable homogeneous.
Described electroplating aqueous solution, wherein graphene oxide concentration is 0.5 ~ 5 mg/ml, and conductive polymer concentration is 0.01 ~ 0.5 mol/L, makes electroplating solution moderate concentration.
The described nitrogen that is blown in aqueous solution refers to and is blown into nitrogen more than ten minutes, discharges wherein oxygen, to prevent conducting polymer monomer oxidized in the solution.
The described electroplated electrode that needs refers to metal, graphite, electro-conductive glass, conducting polymer or conducting metal oxide, selects according to purposes and demand.
Described refers to platinum foil (net), native gold (net), precious metal alloys sheet (net), stainless steel substrates (net) or glass-carbon electrode to electrode, is in electrochemical process not occur the inert material of redox reaction.
Described immersion plating solution refers to by needs electroplated electrode with electrode is perpendicular to ground and parallel is relatively placed in electroplating solution, form uniform and stable electric force lines distribution in the electrolytic solution.
Described a period of time refers to 50 ~ 5000 seconds, and the thickness of coating making formation is moderate.
Described plating refers to constant voltage plating or constant current plating, and constant voltage electroplating voltage ranges for 0.5 ~ 1.5 volt, and constant current electroplating current density is 0.05 ~ 5 milliampere/square centimeter, makes generation electrochemical reaction moderate strength.
The present invention prepares graphene oxide/conducting polymer composite deposite by said method, conducting polymer monomer forms polymer long-chain by electrochemical oxidation, in graphene oxide, electronegative group institute on conducting polymer long-chain positively charged is combined by ionic bond, and co-deposition covers needs electroplated electrode surface.Wherein, graphene oxide monoatomic layer, as structural material, interts and is distributed in composite deposite, form unordered overlapping three-dimensional internet network structure；Conducting polymer, as functional material, is filled in the middle of graphene oxide network, forms firm electric charge transmission coating.
By the composite deposite stable homogeneous that the present invention prepares, coating shape, size and thickness can need the electrical quantity of electroplated electrode geomery and electroplating solution concentration proportioning and plating and time parameter change and control by change.Prepared composite deposite has bigger specific surface area so that the plating impedance reduction of electrode of coating, electric charge transmission electric capacity increase；Owing to graphene oxide has superior mechanical performance, the stability that coating has had；Coating has good biocompatibility simultaneously.Comprehensive above characteristic, prepared graphene oxide/conducting polymer composite deposite can be made implantating biological medical-treatment electrode equipment.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of prepared graphene oxide/Polyglycolic acid fibre (PEDOT) composite deposite.
Fig. 2 is the AC impedance correlation curve of the gold electrode of gold electrode and the modification of graphene oxide/Polyglycolic acid fibre (PEDOT) composite deposite.
Fig. 3 is the cyclic voltammetric correlation curve of the gold electrode of gold electrode and the modification of graphene oxide/Polyglycolic acid fibre (PEDOT) composite deposite.
Detailed description of the invention
Below in conjunction with accompanying drawing, embodiments of the invention are elaborated: the present embodiment is carried out under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
1. weigh carboxylated Graphene 100 milligrams, add 100 ml deionized water, carboxylated graphene aqueous solution adds 0.001 mole of 3,4-ethylene dioxythiophene (EDOT) monomer；
2. solution is placed in ultra-sonic washer ultrasonic half an hour, rotating speed 400 revs/min is used to stir one hour, be made into carboxylated Graphene concentration be 1 mg/ml, 3,4-ethylenedioxy thiophene (EDOT) monomer concentration is the electroplating solution of 0.01 mol/L, in electroplating solution, it is blown into nitrogen ten minutes, discharges wherein oxygen；
3., by needing the gold electrode electroplated with platinum foil to, in electrode vertically relative immersion plating solution, connecting positive source and negative pole respectively, use constant current plating, set electric current density as 0.2 milliampere/square centimeter, sedimentation time 1800 seconds；
4. from electroplating solution, take out gold electrode, use deionized water rinsing gold electrode surfaces, namely obtain carboxylation Graphene/Polyglycolic acid fibre (PEDOT) composite deposite covering on gold electrode.
Embodiment 2
1. weigh graphene oxide 500 milligrams, add 100 ml deionized water, graphene oxide water solution adds 0.05 mole of pyrroles (Py) monomer；
2. solution is placed in ultra-sonic washer ultrasonic half an hour, rotating speed 600 revs/min is used to stir one hour, it is made into carboxylation Graphene concentration to be 5 mg/ml, pyrroles (Py) monomer concentration is the electroplating solution of 0.5 mol/L, in electroplating solution, it is blown into nitrogen 20 minutes, discharges wherein oxygen；
3., by needing the conductive glass electrode electroplated with glass-carbon electrode to, in electrode vertically relative immersion plating solution, connecting positive source and negative pole respectively, use constant current plating, set electric current density as 0.05 milliampere/square centimeter, sedimentation time 5000 seconds；
4. from electroplating solution, take out conductive glass electrode, use deionized water rinsing conductive glass electrode surface, namely obtain graphene oxide/polypyrrole (PPy) composite deposite covering on conductive glass electrode.
Embodiment 3
1. weigh graphene oxide 50 milligrams, add 100 ml deionized water, graphene oxide water solution adds 0.01 mole of thiophene (Th) monomer；
2. solution is placed in ultra-sonic washer ultrasonic half an hour, rotating speed 500 revs/min is used to stir one hour, it is made into carboxylation Graphene concentration to be 0.5 mg/ml, thiophene (Th) monomer concentration is the electroplating solution of 0.1 mol/L, in electroplating solution, it is blown into nitrogen ten minutes, discharges wherein oxygen；
3., by needing the platinum electrode electroplated with stainless steel substrates to, in electrode vertically relative immersion plating solution, connecting positive source and negative pole respectively, use constant current plating, set electric current density as 5 milliamperes/square centimeter, sedimentation time 50 seconds；
4. from electroplating solution, take out platinum electrode, use deionized water rinsing platinum electrode surface, namely obtain graphene oxide/polythiophene (PTh) composite deposite covering on platinum electrode.
Embodiment 4
1. weigh graphene oxide 200 milligrams, add 100 ml deionized water, graphene oxide water solution adds 0.005 mole aniline (An) monomer；
2. solution is placed in ultra-sonic washer ultrasonic half an hour, rotating speed 550 revs/min is used to stir one hour, it is made into carboxylation Graphene concentration to be 2 mg/ml, aniline (An) monomer concentration is the electroplating solution of 0.05 mol/L, in electroplating solution, it is blown into nitrogen ten minutes, discharges wherein oxygen；
3. by needing the iridium electrode electroplated with native gold to, in electrode vertically relative immersion plating solution, connecting positive source and negative pole respectively, using constant voltage plating, setting voltage is 1.5 volts, sedimentation time 300 seconds；
4. from electroplating solution, take out iridium electrode, use deionized water rinsing iridium electrode surface, namely obtain graphene oxide/polyaniline (PAn) composite deposite covering on iridium electrode.
Embodiment 5
1. weigh graphene oxide 100 milligrams, add 100 ml deionized water, graphene oxide water solution adds 0.01 mole of thiophene (Th) monomer；
2. solution is placed in ultra-sonic washer ultrasonic half an hour, rotating speed 500 revs/min is used to stir one hour, it is made into carboxylation Graphene concentration to be 1 mg/ml, thiophene (Th) monomer concentration is the electroplating solution of 0.1 mol/L, in electroplating solution, it is blown into nitrogen ten minutes, discharges wherein oxygen；
3. by needing the graphite electrode electroplated with platinum titanium alloy reticulated to, in electrode vertically relative immersion plating solution, connecting positive source and negative pole respectively, using constant voltage plating, setting voltage is 0.5 volt, sedimentation time 2400 seconds；
4. from electroplating solution, take out graphite electrode, use deionized water rinsing graphite electrode surface, namely obtain graphene oxide/polythiophene (PTh) composite deposite covering on graphite electrode.
As Figure 1-3:
Fig. 1 is the electron scanning micrograph of prepared graphene oxide/Polyglycolic acid fibre (PEDOT) composite deposite.
Fig. 2 is the AC impedance correlation curve of the gold electrode of gold electrode and the modification of graphene oxide/Polyglycolic acid fibre (PEDOT) composite deposite, and modified rear electrode impedance reduces in whole frequency range.
Fig. 3 is the cyclic voltammetric correlation curve of the gold electrode of gold electrode and the modification of graphene oxide/Polyglycolic acid fibre (PEDOT) composite deposite, and the electric charge transmission electric capacity of modified rear electrode is greatly increased.
Although present disclosure has been made to be discussed in detail already by above preferred embodiment, but it should be appreciated that the description above is not considered as limitation of the present invention.After those skilled in the art have read foregoing, multiple amendment and replacement for the present invention all will be apparent from.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (7)
1. the preparation method of graphene oxide/conducting polymer composite deposite, it is characterised in that be made up of following steps:
First weigh graphene oxide and conducting polymer monomer to add in scrubbing water, utilize ultrasonic and stirring to be made into electroplating aqueous solution, in aqueous solution, be blown into nitrogen prevent monomer oxidation；
Then by needing the electrode of plating and in electrode immersion plating solution, connecing positive source and negative pole respectively, electroplating through after a while is needing the coating that on electroplated electrode, formation graphene oxide and conducting polymer uniformly mix；
Described graphene oxide refer to carboxyl, hydroxyl, sulfonic group, epoxy radicals negative charge group Graphene；
Described conducting polymer monomer refers in thiophene, pyrroles, aniline and derivatives thereof a kind of；
Described electroplating aqueous solution refers to that graphene oxide concentration is 0.5～5 mg/ml, and conductive polymer concentration is 0.01～0.5 mol/L；
The described electroplated electrode that needs refers to metal, graphite, electro-conductive glass, conducting polymer and conducting metal oxide；
Described refers to platinum foil or net, native gold or net, precious metal alloys sheet or net, stainless steel substrates or net and glass-carbon electrode to electrode；
Described immersion plating solution refers to needs electroplated electrode is placed in electroplating solution with to electrode is vertically relative；
Described a period of time refers to 50～5000 seconds；
Described plating refers to constant voltage plating or constant current plating, and constant voltage electroplating voltage ranges for 0.5～1.5 volt, and constant current electroplating current density is 0.05～5 milliampere/square centimeter；
Described conducting polymer monomer forms polymer long-chain by electrochemical oxidation, in graphene oxide, electronegative group institute on conducting polymer long-chain positively charged is combined by ionic bond, co-deposition covers needs electroplated electrode surface, wherein, graphene oxide monoatomic layer is as structural material, interting is distributed in composite deposite, forms unordered overlapping three-dimensional internet network structure；Conducting polymer, as functional material, is filled in the middle of graphene oxide network, forms firm electric charge transmission coating.
2. the preparation method of graphene oxide according to claim 1/conducting polymer composite deposite, is characterized in that, described scrubbing water refers to deionized water or ultra-pure water.
3. the preparation method of graphene oxide according to claim 1/conducting polymer composite deposite, it is characterized in that, described ultrasonic refer to be placed in ultrasonic cleaner by the mixed solution container filling graphene oxide, conducting polymer monomer and scrubbing water ultrasonic half an hour more than.
4. the preparation method of graphene oxide according to claim 1/conducting polymer composite deposite, is characterized in that, described stirring refers to that rotating speed stirs mixed liquor more than one hour more than 100 revs/min, forms the electroplating aqueous solution of stable homogeneous.
5. the preparation method of graphene oxide according to claim 1/conducting polymer composite deposite, is characterized in that, described thiophene is 3,4-ethylene dioxythiophene.
6. the preparation method of the graphene oxide according to any one of claim 1-5/conducting polymer composite deposite, it is characterized in that, the described nitrogen that is blown in aqueous solution refers to and is blown into nitrogen more than ten minutes, discharges wherein oxygen, to prevent conducting polymer monomer oxidized in the solution.
7. graphene oxide/conducting polymer composite deposite that method according to any one of claim 1-6 obtains, it is characterized in that, described conducting polymer monomer forms polymer long-chain by electrochemical oxidation, in graphene oxide, electronegative group institute on conducting polymer long-chain positively charged is combined by ionic bond, co-deposition covers needs electroplated electrode surface, wherein, graphene oxide monoatomic layer is as structural material, interting is distributed in composite deposite, forms unordered overlapping three-dimensional internet network structure；Conducting polymer, as functional material, is filled in the middle of graphene oxide network, forms firm electric charge transmission coating.
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