CN102817057A - Graphene oxide/conducting polymer composite coating and preparation method thereof - Google Patents
Graphene oxide/conducting polymer composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene oxide/conducting polymer composite coating and a preparation method thereof. The preparation method comprises the following steps of weighing graphene oxide and a conducting polymer monomer, adding the graphene oxide and the conducting polymer monomers into purified water, carrying out ultrasonic stirring to obtain a plating solution, blowing nitrogen into the plating solution so that oxygen in the plating solution is removed, immersing an electrode needing plating and a counter electrode in the plating solution, connecting the electrode and the counter electrode respectively to a power positive pole and a power negative pole, and carrying out plating for a period of time so that a uniform layer of the graphene oxide/conducting polymer composite coating is formed on the electrode needing plating. The graphene oxide/conducting polymer composite coating is uniform and stable, has good electrical properties, stability and biocompatibility and can be used for manufacture of implantable biomedical equipment.
Description
Technical field
What the present invention relates to is the composite deposite in a kind of biomedical engineering technology field and preparation method thereof, specifically is graphene oxide/conductive polymers composite deposite and preparation method thereof.
Background technology
Use the implantating biological microelectrode can implement functional electrical stimulation or physiology electric record.As electricity device and biological tissue's interface, the electrode points decorative material is the key factor of decision biological microelectrode performance.Can work safely and effectively for guaranteeing that biological microelectrode is implanted in the live body, the electrode points decorative material should have good following properties: chemical property, i.e. low resistance and big electric charge injection capacity; Stability promptly still keeps excellent electrochemical properties through being repeatedly used; Biocompatibility can not cause biological rejection or tissue necrosis after promptly implanting.
Conductive polymers has many-sided excellent characteristic, for example can mix through difference and carry out varied modification, excellent biological compatibility and excellent electrochemical properties easily, thereby be widely used in a plurality of fields in the last few years.Emerging nano material Graphene because of it constantly shows the excellent performance of each side, and becomes the focus of research now.Utilize graphene oxide as counter ion and conductive polymers composite deposite,, satisfy each item requirement as the electrode points decorative material in conjunction with both high-performances through electrochemical synthesis.Its preparation process is simple and cost is low, is easy to carry out modification according to different performance demand change raw material type and proportioning.
Retrieval through to the prior art document is found; Kip A Ludwig; Nicholas B Langhals etc. writes articles " Poly (3; 4-ethylenedioxythiophene) (PEDOT) polymer coatings facilitate smaller neural recording electrodes " (" gather (3,4-enedioxy thiophene) (PEDOT) polymer coating promote littler neural recording electrode " " neural engineering periodical ") at JOURNAL OF NEURAL ENGINEERING.8 (2011) 014001.The preparation and the measuring technology of the nerve electrode that a kind of conductive polymers PEDOT coating is modified have been mentioned in the document.This technology at the synthetic PEDOT of electrode points surface electrochemistry, is improved the electric property of electrode through the continuous current method.Its shortcoming is to use perchlorate not good as the polymer coating stability of counter ion.The coating pattern can change after a large amount of multiple electricity irritation of long period or electric record, in addition the cracking or peel off.This can influence the electric property of electrode greatly, and small coating spall might remain in the bodily tissue, and the danger of the Health hazard of causing is arranged.Therefore, this conductive polymers coating is not suitable for being used for making the electric physiological apparatus of long-term implantable bioartificial medical treatment.
Summary of the invention
The present invention is directed to the above-mentioned deficiency that prior art exists, a kind of graphene oxide/conductive polymers composite deposite and preparation method thereof is provided.Use the electric property of the bioelectrode that this composite deposite modifies to improve greatly, and coating has good stability and biocompatibility, can be used to make the implantating biological medical facilities.Its making processes is simple to operation, and utilizes electrochemical method for synthesizing to be easy to control coating shape, size and performance.Overall cost of manufacture is low, is beneficial to a large amount of preparations.
The present invention realizes through following technical scheme:
At first weighing graphene oxide and conductive polymers monomer add and to purify waste water, and utilize ultrasonicly to be made into electroplating aqueous solution with stirring, in the aqueous solution, are blown into nitrogen and prevent the monomer oxidation;
Then need galvanized electrode and counter electrode immersion plating solution in, connect positive source and negative pole respectively, electroplate through after a while and on the need electroplated electrode, form graphene oxide and the even miscellaneous coating of conductive polymers.
Described graphene oxide is meant the Graphene of negative charge groups such as having carboxyl, hydroxyl, sulfonic group, epoxy group(ing), and it has water dispersible preferably.
Described conductive polymers monomer is meant 3, and is a kind of in 4-enedioxy thiophene (EDOT), thiophene (Th), pyrroles (Py), aniline (An) and above each monomeric growth.
Described purifying waste water is meant deionized water or ultrapure water.
Described ultrasonic being meant places ultrasonic cleaner ultrasonic above half a hour the mixed solution container that fills graphene oxide, conductive polymers monomer and purify waste water, and forms uniform graphene oxide dispersion liquid.
Described stirring is meant that rotating speed mixes liquid greater than 100 rev/mins and surpasses one hour, forms the electroplating aqueous solution of stable homogeneous.
Described electroplating aqueous solution, wherein graphene oxide concentration is 0.5 ~ 5 mg/ml, the conducting polymer substrate concentration is 0.01 ~ 0.5 mol, makes electroplating solution concentration moderate.
The described nitrogen that in the aqueous solution, is blown into is meant that being blown into nitrogen surpasses ten minutes, discharges wherein oxygen, and is oxidized in solution to prevent the conductive polymers monomer.
The described electroplated electrode that needs is meant metal, graphite, conductive glass, conductive polymers or conducting metal oxide, selects according to purposes and demand.
Described counter electrode is meant platinum foil (net), goldleaf (net), precious metal alloys sheet (net), stainless steel substrates (net) or glass-carbon electrode, is the inert material that redox reaction does not take place in electrochemical process.
Be meant in the described immersion plating solution needs electroplated electrode and counter electrode and in electrolytic solution, form uniform and stable electric force lines distribution perpendicular to ground and parallel being opposite to mutually in the electroplating solution.
Described for some time is meant 50 ~ 5000 seconds, makes the thickness of coating of formation moderate.
Described plating is meant that constant voltage is electroplated or continuous current is electroplated, and constant voltage electroplating voltage scope is 0.5 ~ 1.5 volt, and the continuous current electroplating current density is 0.05 ~ 5 milliampere/square centimeter, makes generation electrochemical reaction intensity moderate.
The present invention obtains graphene oxide/conductive polymers composite deposite through method for preparing; The conductive polymers monomer forms the polymkeric substance long-chain through electrochemical oxidation; Institute is positively charged on electronegative group and the conductive polymers long-chain in the graphene oxide combines through ionic linkage, and it is surperficial that common deposited covers the need electroplated electrode.Wherein, the graphene oxide monoatomic layer is as structured material, and interspersed being distributed in the composite deposite forms the three-dimensional internet network structure of unordered overlapping; Conductive polymers is filled in the middle of the graphene oxide network as functional materials, forms firm charge transfer coating.
Through the composite deposite stable homogeneous that the present invention makes, coating shape, size and thickness can be through change to need electroplated electrode geomery and electroplating solution concentration proportioning and galvanized electrical parameter and time parameter to change and control.Make composite deposite and have bigger specific surface area, feasible impedance reduction, the charge transfer electric capacity of electroplating the electrode of coating increases; Because graphene oxide has superior mechanical property, coating has good stability; Coating has excellent biological compatibility simultaneously.Comprehensive above characteristic, the graphene oxide that makes/conductive polymers composite deposite can be made implantating biological medical-treatment electrode equipment.
Description of drawings
Fig. 1 is the graphene oxide that makes/the gather electron scanning micrograph of enedioxy thiophene (PEDOT) composite deposite.
Fig. 2 is gold electrode and graphene oxide/the gather alternating-current impedance correlation curve of the gold electrode of enedioxy thiophene (PEDOT) composite deposite modification.
Fig. 3 is gold electrode and graphene oxide/the gather cyclic voltammetric correlation curve of the gold electrode of enedioxy thiophene (PEDOT) composite deposite modification.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Embodiment 1
1. take by weighing 100 milligrams of carboxylated Graphenes, add 100 ml deionized water, in carboxylated graphene aqueous solution, add 0.001 mole 3,4-enedioxy thiophene (EDOT) monomer;
2. solution is placed ultra-sonic cleanser ultrasonic half a hour; Use rotating speed to stir one hour for 400 rev/mins; Being made into carboxylated Graphene concentration is 1 mg/ml, 3; 4-enedioxy thiophene (EDOT) monomer concentration is the electroplating solution of 0.01 mol, in electroplating solution, is blown into nitrogen ten minutes, discharges wherein oxygen;
3. need galvanized gold electrode and platinum foil counter electrode vertically relatively in the immersion plating solution, connect positive source and negative pole respectively, use continuous current to electroplate, setting current density is 0.2 milliampere/square centimeter, depositing time 1800 seconds;
4. from electroplating solution, take out gold electrode, use the deionized water rinsing gold electrode surfaces, promptly obtain covering carboxylation Graphene on the gold electrode/gather enedioxy thiophene (PEDOT) composite deposite.
Embodiment 2
1. take by weighing 500 milligrams of graphene oxides, add 100 ml deionized water, in the graphite oxide aqueous solution, add 0.05 mole of pyrroles (Py) monomer;
2. solution is placed ultra-sonic cleanser ultrasonic half a hour; Use rotating speed to stir one hour for 600 rev/mins; Being made into carboxylation Graphene concentration is that 5 mg/ml, pyrroles (Py) monomer concentration are the electroplating solution of 0.5 mol; In electroplating solution, be blown into nitrogen 20 minutes, and discharged wherein oxygen;
3. need galvanized conductive glass electrode and glass-carbon electrode counter electrode vertically relatively in the immersion plating solution, connect positive source and negative pole respectively, use continuous current to electroplate, setting current density is 0.05 milliampere/square centimeter, depositing time 5000 seconds;
4. from electroplating solution, take out conductive glass electrode, use deionized water rinsing conductive glass electrode surface, promptly obtain covering graphene oxide/polypyrrole (PPy) composite deposite on the conductive glass electrode.
Embodiment 3
1. take by weighing 50 milligrams of graphene oxides, add 100 ml deionized water, in the graphite oxide aqueous solution, add 0.01 mole of thiophene (Th) monomer;
2. solution is placed ultra-sonic cleanser ultrasonic half a hour; Use rotating speed to stir one hour for 500 rev/mins; Being made into carboxylation Graphene concentration is that 0.5 mg/ml, thiophene (Th) monomer concentration are the electroplating solution of 0.1 mol; In electroplating solution, be blown into nitrogen ten minutes, and discharged wherein oxygen;
3. need galvanized platinum electrode and stainless steel substrates counter electrode vertically relatively in the immersion plating solution, connect positive source and negative pole respectively, use continuous current to electroplate, setting current density is 5 milliamperes/square centimeter, depositing time 50 seconds;
4. from electroplating solution, take out platinum electrode, use the deionized water rinsing platinum electrode surface, promptly obtain covering graphene oxide/Polythiophene (PTh) composite deposite on the platinum electrode.
Embodiment 4
1. take by weighing 200 milligrams of graphene oxides, add 100 ml deionized water, in the graphite oxide aqueous solution, add 0.005 mole of aniline (An) monomer;
2. solution is placed ultra-sonic cleanser ultrasonic half a hour; Use rotating speed to stir one hour for 550 rev/mins; Being made into carboxylation Graphene concentration is that 2 mg/ml, aniline (An) monomer concentration are the electroplating solution of 0.05 mol; In electroplating solution, be blown into nitrogen ten minutes, and discharged wherein oxygen;
3. need galvanized iridium electrode and goldleaf counter electrode vertically relatively in the immersion plating solution, connect positive source and negative pole respectively, use constant voltage to electroplate, setting voltage is 1.5 volts, depositing time 300 seconds;
4. from electroplating solution, take out iridium electrode, use deionized water rinsing iridium electrode surface, promptly obtain covering graphene oxide/polyaniline (PAn) composite deposite on the iridium electrode.
1. take by weighing 100 milligrams of graphene oxides, add 100 ml deionized water, in the graphite oxide aqueous solution, add 0.01 mole of thiophene (Th) monomer;
2. solution is placed ultra-sonic cleanser ultrasonic half a hour; Use rotating speed to stir one hour for 500 rev/mins; Being made into carboxylation Graphene concentration is that 1 mg/ml, thiophene (Th) monomer concentration are the electroplating solution of 0.1 mol; In electroplating solution, be blown into nitrogen ten minutes, and discharged wherein oxygen;
3. need galvanized Graphite Electrodes and platinum titanium alloy reticulated counter electrode vertically relatively in the immersion plating solution, connect positive source and negative pole respectively, use constant voltage to electroplate, setting voltage is 0.5 volt, depositing time 2400 seconds;
4. from electroplating solution, take out Graphite Electrodes, use the deionized water rinsing graphite electrode surface, promptly obtain covering graphene oxide/Polythiophene (PTh) composite deposite on the Graphite Electrodes.
Shown in Fig. 1-3:
Fig. 1 is the graphene oxide that makes/the gather electron scanning micrograph of enedioxy thiophene (PEDOT) composite deposite.
The alternating-current impedance correlation curve of the gold electrode that Fig. 2 modifies for gold electrode and graphene oxide/gather enedioxy thiophene (PEDOT) composite deposite reduces in whole frequency range through the impedance of modification rear electrode.
The cyclic voltammetric correlation curve of the gold electrode that Fig. 3 modifies for gold electrode and graphene oxide/gather enedioxy thiophene (PEDOT) composite deposite increases through the charge transfer electric capacity of modification rear electrode greatly.
Although content of the present invention has been done detailed introduction through above-mentioned preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be conspicuous.Therefore, protection scope of the present invention should be limited appended claim.
Claims (14)
1. the preparation method of graphene oxide/conductive polymers composite deposite is characterized in that, may further comprise the steps:
At first weighing graphene oxide and conductive polymers monomer add and to purify waste water, and utilize ultrasonicly to be made into electroplating aqueous solution with stirring, in the aqueous solution, are blown into nitrogen and prevent the monomer oxidation;
Then need galvanized electrode and counter electrode immersion plating solution in, connect positive source and negative pole respectively, electroplate through after a while and on the need electroplated electrode, form graphene oxide and the even miscellaneous coating of conductive polymers.
2. the preparation method of graphene oxide according to claim 1/conductive polymers composite deposite is characterized in that, described graphene oxide is meant the Graphene that has carboxyl, hydroxyl, sulfonic group, epoxy group(ing) negative charge group.
3. the preparation method of graphene oxide according to claim 1/conductive polymers composite deposite is characterized in that, described conductive polymers monomer is meant 3, and is a kind of in 4-enedioxy thiophene, thiophene, pyrroles, aniline and the growth thereof.
4. the preparation method of graphene oxide according to claim 1/conductive polymers composite deposite is characterized in that, described purifying waste water is meant deionized water or ultrapure water.
5. the preparation method of graphene oxide according to claim 1/conductive polymers composite deposite; It is characterized in that described ultrasonic being meant places ultrasonic cleaner more than ultrasonic half a hour the mixed solution container that fills graphene oxide, conductive polymers monomer and purify waste water.
6. the preparation method of graphene oxide according to claim 1/conductive polymers composite deposite is characterized in that, described stirring is meant that rotating speed mixes liquid more than one hour greater than 100 rev/mins, forms the electroplating aqueous solution of stable homogeneous.
7. according to the preparation method of each described graphene oxide/conductive polymers composite deposite of claim 1-6; It is characterized in that; Described electroplating aqueous solution is meant that graphene oxide concentration is 0.5 ~ 5 mg/ml, and the conducting polymer substrate concentration is 0.01 ~ 0.5 mol.
8. according to the preparation method of each described graphene oxide/conductive polymers composite deposite of claim 1-6; It is characterized in that; The described nitrogen that in the aqueous solution, is blown into is meant and is blown into nitrogen more than ten minutes, discharges wherein oxygen, and is oxidized in solution to prevent the conductive polymers monomer.
9. according to the preparation method of each described graphene oxide/conductive polymers composite deposite of claim 1-6, it is characterized in that the described electroplated electrode that needs is meant metal, graphite, conductive glass, conductive polymers and conducting metal oxide.
10. according to the preparation method of each described graphene oxide/conductive polymers composite deposite of claim 1-6, it is characterized in that described counter electrode is meant platinum foil or net, goldleaf or net, precious metal alloys sheet or net, stainless steel substrates or net and glass-carbon electrode.
11. the preparation method according to each described graphene oxide/conductive polymers composite deposite of claim 1-6 is characterized in that, is meant in the described immersion plating solution needs electroplated electrode vertically is opposite in the electroplating solution with counter electrode mutually.
12. the preparation method according to each described graphene oxide/conductive polymers composite deposite of claim 1-6 is characterized in that described for some time is meant 50 ~ 5000 seconds.
13. preparation method according to each described graphene oxide/conductive polymers composite deposite of claim 1-6; It is characterized in that; Described plating is meant that constant voltage is electroplated or continuous current is electroplated; Constant voltage electroplating voltage scope is 0.5 ~ 1.5 volt, and the continuous current electroplating current density is 0.05 ~ 5 milliampere/square centimeter.
14. the graphene oxide/conductive polymers composite deposite that obtains according to the said method of claim 1-13; It is characterized in that; Said conductive polymers monomer forms the polymkeric substance long-chain through electrochemical oxidation, and institute is positively charged on electronegative group and the conductive polymers long-chain in the graphene oxide combines through ionic linkage, and common deposited covers need electroplated electrode surperficial; Wherein, The graphene oxide monoatomic layer is as structured material, and interspersed being distributed in the composite deposite forms the three-dimensional internet network structure of unordered overlapping; Conductive polymers is filled in the middle of the graphene oxide network as functional materials, forms firm charge transfer coating.
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