KR102336814B1 - Biocompatible electrode active material and method of manufacturing thereof and super capacitor including the same - Google Patents

Abstract

Disclosed are a biocompatible electrode active material and a method for manufacturing the same, and super capacitor having the same. According to the present invention, the biocompatible electrode active material consists of a compound having ta structure of the following formula 1: ATiOPO_4 (where [A] is Na or K).

Description

Biocompatible electrode active material, manufacturing method thereof, and supercapacitor having the same

The present invention relates to a biocompatible electrode active material, a method for producing the same, and a supercapacitor having the same, and more particularly, to a biocompatible electrode active material having biocompatible properties and a method for producing the same, and a supercapacitor having the same It's about capacitors.

Among next-generation energy storage devices, supercapacitors are in the spotlight as a next-generation energy storage device due to their fast charging/discharging speed, high stability, and eco-friendly characteristics. A typical supercapacitor is composed of a porous electrode, a current collector, a separator, and an electrolyte.

Supercapacitors are also referred to as Electric Double Layer Capacitors (EDLC) or Ultra-capacitors, which are a pair of charge layers ( It is a device that does not require maintenance because deterioration due to repeated charging/discharging operations is very small. Accordingly, supercapacitors are mainly used in the form of backing up IC (integrated circuit) of various electric and electronic devices, and their use has recently been expanded to toys, solar energy storage, HEV (hybrid electric vehicle) power supply, bio-inserted medical devices It has been widely applied to supercapacitors for equipment, etc.

Such a supercapacitor generally includes two electrodes of an anode and a cathode impregnated with an electrolyte, and a separator of a porous material that is interposed between these two electrodes to allow only ion conduction and to prevent insulation and short circuit, and the electrolyte; It has a unit cell composed of a gasket for preventing leakage and insulation and short circuit, and a metal cap as a conductor for packaging them. And it is completed by stacking one or more unit cells (usually, 2 to 6 in case of coin type) configured as above in series and combining the two terminals of the positive and negative electrodes.

The performance of a supercapacitor is determined by the electrode active material and electrolyte, and in particular, the main performance such as capacitance is mostly determined by the electrode active material. Recently, in order to manufacture a supercapacitor that can operate stably even at a high voltage, development of core material technology for capacitor components such as an electrode active material suitable for a high voltage, an electrolyte, and a sealing material is being actively conducted.

The inventors of the present invention tried to develop an electrode active material that is accompanied by an electrochemical reaction and has biocompatible properties and applied it to a supercapacitor for a medical device inserted into the human body.

As a related prior document, there is Republic of Korea Patent Registration No. 10-1734822 (published on May 12, 2017), which describes an in vivo energy storage system and an in vivo energy storage method using the same.

SUMMARY OF THE INVENTION It is an object of the present invention to provide a biocompatible electrode active material accompanied by an electrochemical reaction and having biocompatible properties, a method for manufacturing the same, and a supercapacitor having the same.

A biocompatible electrode active material according to an embodiment of the present invention for achieving the above object is characterized in that it consists of a compound having a structure of the following [Formula 1].

[Formula 1]: ATiOPO ₄

(Where [A] is Na or K.)

By having the structure of the above [Formula 1], it is used as an electrode active material of a supercapacitor through an electrochemical reaction in a body fluid.

In addition, the electrode active material further includes at least one carbon material selected from carbon nanotubes, carbon nanofibers, graphene, and activated carbon, and can be composited by mixing with the carbon material.

In addition, the electrode active material is accompanied by an electrochemical reaction in an electrolyte containing Na or K.

Here, the electrolyte is MClO ₄ , MBF ₄ , MPF ₆ , MTFSI, MFSI and MSO ₄ (where M is Na or K.) An electrolyte salt comprising at least one selected from, and a solvent for dissolving the electrolyte salt includes

In addition, the solvent is ethylene carbonate (EC), propylene carbonate (PC), fluoroethylene carbonate (FEC), dimethyl carboenite (DMC), diethyl carbonate (DEC), dimethyl carbonate (EMC), dimethoxyethane ( DME), tetraethylene glycol dimethyl ether (TEGDME), diethylene glycol dimethyl ether (DEGDME), and may include one or more selected from water.

A method for preparing a biocompatible electrode active material according to an embodiment of the present invention for achieving the above object includes the steps of: _{(a) synthesizing Na 4} TiPO _{4 as a starting material;} (b) _{mixing the synthesized Na 4} TiPO ₄ with potassium nitrate or sodium nitrate and bathing at 80 to 120° C., followed by stirring; And (c) the resultant of step (b) is stirred while heating to 250 ~ 350 ℃, neutralized until pH 6.5 ~ 7.5 using distilled water, filtered and dried to a compound having a structure of the following formula (1) It characterized in that it comprises; obtaining an electrode active material consisting of.

[Formula 1]: ATiOPO ₄

(Where [A] is Na or K.)

Here, the step (a) is, (a-1) _{after dissolving Ti(SO 4} ) ₂ in distilled water, _{adding H 3} PO ₄ and NH ₃ H ₂ O and stirring for 5 to 7 hours; (a-2) microwave-treating the stirred resultant into a microwave container; And (a-3) the resultant mask wave treatment is stirred in distilled water, washed until pH is 6.5 to 7.5, filtered, and dried at 100 to 140° C. for 20 to 30 hours to obtain _{Na 4} TiPO _{4 .} step; includes.

The microwave treatment is preferably performed for 10 to 30 minutes under conditions of 350 to 450W and 250 to 350 psi.

In step (b), the Na ₄ TiPO ₄ and potassium nitrate or sodium nitrate is preferably mixed in a weight ratio of 1: 2 to 1: 4.

In step (c), the drying is carried out at 100 ~ 140 ℃ for 20 ~ 30 hours.

In a supercapacitor having a biocompatible electrode active material according to an embodiment of the present invention for achieving the above object, the positive electrode and the negative electrode are spaced apart from each other, and between the positive electrode and the negative electrode, to prevent a short circuit between the positive electrode and the negative electrode A separator is disposed for the anode and the cathode are impregnated in the electrolyte of the supercapacitor,

Each of the positive and negative electrodes includes an electrode active material, a conductive material and a binder,

At least one of the electrode active material of the positive electrode and the negative electrode,

It is characterized in that it consists of a compound having the structure of the following [Formula 1].

[Formula 1]: ATiOPO ₄

(Where [A] is Na or K.)

In this case, the electrolyte is MClO ₄ , MBF ₄ , MPF ₆ , MTFSI, MFSI and MSO ₄ (where M is Na or K.) An electrolyte salt comprising at least one selected from, and a solvent for dissolving the electrolyte salt includes

In addition, the solvent is ethylene carbonate (EC), propylene carbonate (PC), fluoroethylene carbonate (FEC), dimethyl carboenite (DMC), diethyl carbonate (DEC), dimethyl carbonate (EMC), dimethoxyethane ( DME), tetraethylene glycol dimethyl ether (TEGDME), diethylene glycol dimethyl ether (DEGDME), and may include one or more selected from water.

The biocompatible electrode active material according to the present invention is _{composed of a compound having a structure of NaTiOPO 4} or KTiOPO ₄ , and thus accompanies an electrochemical reaction in a body fluid, and has excellent biocompatibility with low toxicity to the living body.

As a result, since the biocompatible electrode active material according to the present invention has excellent biocompatibility due to low toxicity to the living body, the MTT assay (cell proliferation and apoptosis change) test result of the supercapacitor electrode showed 90 in the cell viability test for more than 3 days. It was confirmed that the cell viability of % or more was exhibited.

In addition, since the biocompatible electrode active material according to the present invention has little toxicity to the living body, it can be applied to an energy storage device for an implantable medical device.

Therefore, when the biocompatible electrode active material according to the present invention is used as an electrode active material for a positive electrode and a negative electrode for a supercapacitor, it has excellent biocompatibility, so that it is possible to provide a supercapacitor that can be applied to a medical device inserted into a living body and the like.

1 is a process flow chart showing a method for manufacturing a biocompatible electrode active material according to an embodiment of the present invention.
Figure 2 is a process flow chart showing a method of manufacturing a supercapacitor according to an embodiment of the present invention.
3 is a graph showing the cell viability test results for a supercapacitor having a biocompatible electrode active material prepared according to Examples 1 and 2;

Advantages and features of the present invention, and methods for achieving them, will become apparent with reference to the embodiments described below in detail in conjunction with the accompanying drawings. However, the present invention is not limited to the embodiments disclosed below, but will be implemented in a variety of different forms, only this embodiment allows the disclosure of the present invention to be complete, and common knowledge in the technical field to which the present invention belongs It is provided to fully inform the possessor of the scope of the invention, and the present invention is only defined by the scope of the claims. Like reference numerals refer to like elements throughout.

Hereinafter, with reference to the accompanying drawings, a biocompatible electrode active material according to a preferred embodiment of the present invention, a method for manufacturing the same, and a supercapacitor having the same will be described in detail as follows.

The biocompatible electrode active material according to an embodiment of the present invention accompanies an electrochemical reaction and has biocompatible properties.

To this end, the biocompatible electrode active material according to an embodiment of the present invention consists of a compound having the structure of the following [Formula 1].

[Formula 1]: ATiOPO ₄

Here, [A] is Na or K.

That is, the biocompatible electrode active material according to an embodiment of the present invention is a compound having a structure _{of NaTiOPO 4} or KTiOPO _{4 .}

The biocompatible electrode active material according to an embodiment of the present invention is used as an electrode active material of a supercapacitor through an electrochemical reaction in a body fluid by having the structure of the above [Formula 1].

As described above, the biocompatible electrode active material according to an embodiment of the present invention is _{composed of a compound having a structure of NaTiOPO 4} or KTiOPO ₄ , and is accompanied by an electrochemical reaction in a body fluid, and has excellent biocompatibility with low toxicity to the living body. have

As a result, since the biocompatible electrode active material according to an embodiment of the present invention has excellent biocompatibility with low toxicity to the living body, the MTT assay (cell proliferation and apoptosis change) test result of the supercapacitor electrode results in a cell viability of 3 days or more It becomes possible to show a cell viability of more than 90% in the test.

In addition, the biocompatible electrode active material according to an embodiment of the present invention further includes one or more carbon materials selected from carbon nanotubes, carbon nanofibers, graphene, and activated carbon, and can be composited by mixing with the carbon material.

The biocompatible electrode active material according to an embodiment of the present invention involves an electrochemical reaction in an electrolyte containing Na or K.

To this end, the electrolyte is MClO ₄ , MBF ₄ , MPF ₆ , MTFSI, MFSI and MSO ₄ (where M is Na or K.) An electrolyte salt comprising at least one selected from, and a solvent dissolving the electrolyte salt include

At this time, the solvent is ethylene carbonate (EC), propylene carbonate (PC), fluoroethylene carbonate (FEC), dimethyl carboenite (DMC), diethyl carbonate (DEC), dimethyl carbonate (EMC), dimethoxyethane (DME) ), tetraethylene glycol dimethyl ether (TEGDME), diethylene glycol dimethyl ether (DEGDME), and water.

The biocompatible electrode active material according to an embodiment of the present invention is _{composed of a compound having a structure of NaTiOPO 4} or KTiOPO ₄ , and is accompanied by an electrochemical reaction in a body fluid, and has excellent biocompatibility with low toxicity to the living body.

As a result, since the biocompatible electrode active material according to an embodiment of the present invention has excellent biocompatibility with low toxicity to the living body, the MTT assay (cell proliferation and apoptosis change) test result of the supercapacitor electrode results in a cell viability of 3 days or more It was confirmed that the test exhibited a cell viability of 90% or more.

In addition, since the biocompatible electrode active material according to an embodiment of the present invention has little toxicity to the living body, it can be applied to an energy storage device for a medical device inserted into a living body.

Therefore, when the biocompatible electrode active material according to an embodiment of the present invention is used as an electrode active material for a positive electrode and a negative electrode for a supercapacitor, it has excellent biocompatibility, so that it is possible to provide a supercapacitor that can be applied to a bio-inserted medical device.

Hereinafter, a method for manufacturing a biocompatible electrode active material according to an embodiment of the present invention will be described with reference to the accompanying drawings.

1 is a process flow chart showing a method for manufacturing a biocompatible electrode active material according to an embodiment of the present invention.

Referring to FIG. 1 , the method for manufacturing a biocompatible electrode active material according to an embodiment of the present invention includes a starting material synthesis step (S10), a mixing and bathing step (S20), and a heating and drying step (S30).

starting material synthesis

In the starting material synthesis step (S10), the starting material Na ₄ TiPO ₄ is synthesized.

In this step, the process of synthesizing the _{starting material Na 4} TiPO _{4 is as follows.}

First, Ti(SO ₄ ) ₂ After completely dissolving in distilled water, H ₃ PO ₄ and NH ₃ H ₂ O are added and stirred for 5 to 7 hours.

Here, the stirring is preferably performed for 5 to 7 hours at a speed of 1,000 to 3,000 rpm. If the stirring speed is less than 1,000 rpm or the stirring time is less than 5 hours, there is a fear that uniform mixing between the starting materials may not be achieved. Conversely, when the stirring speed exceeds 3,000 rpm or the stirring time exceeds 7 hours, it may act as a factor to increase the manufacturing cost without any further effect, so it is not economical.

Next, the stirred resultant is put into a microwave container and subjected to microwave treatment.

Here, the microwave treatment is preferably carried out for 10 to 30 minutes under conditions of 350 ~ 450W and 250 ~ 350psi.

If the microwave treatment time is less than 10 minutes, there is a fear that sufficient drying may not be achieved. Conversely, when the microwave treatment time exceeds 30 minutes, it is not economical because it may act as a factor increasing only the manufacturing time and cost without further increasing the effect.

Next, the resultant mask wave treatment is stirred in distilled water, washed until the pH is 6.5 to 7.5, filtered, and dried at 100 to 140° C. for 20 to 30 hours to obtain _{Na 4} TiPO _{4 as a starting material.}

mixing and bathing

In the mixing and bathing step (S20), the synthesized Na _{4 TiPO 4} is mixed with potassium nitrate or sodium nitrate and bathed at 80 to 120° C., followed by stirring.

In this step, Na ₄ TiPO ₄ and potassium nitrate or sodium nitrate may be mixed with distilled water.

Here, Na ₄ TiPO ₄ and potassium nitrate or sodium nitrate is preferably mixed in a weight ratio of 1: 2 to 1: 4. When _{the weight ratio of Na 4} TiPO ₄ and potassium nitrate or sodium nitrate is out of the above range, the production cost may increase due to an increase in the amount _{of Na 4} TiPO _{4 , which is not preferable.}

heating and drying

In the heating and drying step (S30), the resultant of the mixing and bathing step (S20) is stirred while heating to 250 ~ 350 ℃, neutralized using distilled water until the pH is 6.5 ~ 7.5, filtered and dried to obtain the following formula An electrode active material composed of a compound having the structure of 1 is obtained.

[Formula 1]: ATiOPO ₄

Here, [A] is Na or K.

As described above, the biocompatible electrode active material prepared by the method according to an embodiment of the present invention is _{composed of a compound having a structure of NaTiOPO 4} or KTiOPO ₄ , and is accompanied by an electrochemical reaction in a body fluid, and has low toxicity to the living body. It has excellent biocompatibility.

As a result, since the biocompatible electrode active material prepared by the method according to the embodiment of the present invention has excellent biocompatibility with little toxicity to the living body, MTT assay (cell proliferation and apoptosis change evaluation) test result 3 of the supercapacitor electrode Cell viability of more than 90% can be exhibited in more than one day cell viability test.

In this step, drying is preferably carried out at 100 ~ 140 ℃ for 20 ~ 30 hours. If the drying temperature is less than 100° C. or the drying time is less than 20 hours, sufficient drying may not be achieved, and thus it may be difficult to secure strength. Conversely, when the drying temperature exceeds 140° C. or the drying time exceeds 30 hours, this is not economical because it may act as a factor that increases only the manufacturing cost without increasing the effect.

As described above, the method for manufacturing a biocompatible electrode active material according to an embodiment of the present invention may be completed.

The biocompatible electrode active material according to an embodiment of the present invention prepared by the above-described method is _{composed of a compound having a structure of NaTiOPO 4} or KTiOPO ₄ , and is accompanied by an electrochemical reaction in a body fluid, and has low toxicity to the living body. It has excellent biocompatibility.

As a result, since the biocompatible electrode active material prepared by the method according to the embodiment of the present invention has excellent biocompatibility with low toxicity to the living body, MTT assay (cell proliferation and apoptosis change evaluation) test result 3 of the supercapacitor electrode Cell viability of more than 90% is shown in a cell viability test of more than one day.

In addition, since the biocompatible electrode active material manufactured by the method according to the embodiment of the present invention has low toxicity to the living body, it can be applied to an energy storage device for an implantable medical device.

Therefore, when the biocompatible electrode active material prepared by the method according to the embodiment of the present invention is used as an electrode active material for a positive electrode and a negative electrode for a supercapacitor, it has excellent biocompatibility, so a supercapacitor that can be applied to a bio-inserted medical device, etc. is provided. can do.

Supercapacitor and manufacturing method thereof

2 is a process flowchart illustrating a method of manufacturing a supercapacitor according to an embodiment of the present invention.

As shown in Figure 2, the supercapacitor manufacturing method according to the embodiment of the present invention is a supercapacitor electrode composition forming step (S110), an electrode form forming step (S120), a supercapacitor electrode forming step (S130), and an electrolyte solution It includes an impregnation step (S140).

Formation of composition for supercapacitor electrode

In the step of forming the composition for a supercapacitor electrode ( S110 ), a composition for a supercapacitor electrode is prepared by mixing an electrode active material, a conductive material, a binder, and a dispersion medium.

A composition for a supercapacitor electrode including an electrode active material, a conductive material, a binder, and a dispersion medium is prepared.

The composition for a supercapacitor electrode contains 2 to 20 parts by weight of the conductive material based on 100 parts by weight of the electrode active material and the electrode active material, 2 to 20 parts by weight of the binder based on 100 parts by weight of the electrode active material, and 200 to 300 parts by weight of the dispersion medium based on 100 parts by weight of the electrode active material. It is preferable to include wealth.

Since such a composition for supercapacitor electrodes is in a doughy state, it may be difficult to uniformly mix (completely disperse). Using a mixer such as a planetary mixer for a predetermined time (eg, 10 minutes to 12 hours) If stirred for a while, a composition for a supercapacitor electrode suitable for electrode manufacturing can be obtained. A mixer such as a planetary mixer enables the preparation of a uniformly mixed composition for a supercapacitor electrode.

As the electrode active material, the biocompatible electrode active material described above is used. That is, the electrode active material is composed of a compound having a structure _{of NaTiOPO 4} or KTiOPO _{4 .} Accordingly, the electrode active material accompanies an electrochemical reaction in the body fluid and has excellent biocompatibility with low toxicity to the living body.

In addition, the electrode active material further includes at least one carbon material selected from carbon nanotubes, carbon nanofibers, graphene, and activated carbon, and can be composited by mixing with the carbon material.

The binder is polytetrafluoroethylene (PTFE; polytetrafluoroethylene), polyvinylidene fluoride (PVdF; polyvinylidenefloride), carboxymethylcellulose (CMC; carboxymethylcellulose), polyvinyl alcohol (PVA; polyvinyl alcohol), polyvinyl butyral (PVB) ; polyvinyl butyral), polyvinylpyrrolidone (PVP; poly-N-vinylpyrrolidone), styrene butadiene rubber (SBR), polyamide-imide, polyimide, etc. One selected type or a mixture of two or more types may be used.

The conductive material is not particularly limited as long as it is an electronically conductive material that does not cause chemical change, and examples include natural graphite, artificial graphite, carbon black, acetylene black, Ketjen black, Super-P black, carbon fiber, copper, nickel, A metal powder, such as aluminum, silver, or a metal fiber, etc. are possible.

The dispersion medium may be an organic solvent such as ethanol (EtOH), acetone, isopropyl alcohol, N-methylpyrrolidone (NMP), propylene glycol (PG), or water.

formed in the form of an electrode

In the electrode form forming step (S120), the supercapacitor electrode composition is compressed to form an electrode form, or the supercapacitor electrode composition is coated on a metal foil to form an electrode form, or the supercapacitor electrode composition is pressed with a roller to form a sheet It is made into a state of being and attached to a metal foil or a current collector to form an electrode.

When explaining the example of the step of forming in the form of an electrode in more detail, the composition for a supercapacitor electrode may be molded by compression using a roll press molding machine. The roll press molding machine aims to improve the electrode density and control the thickness of the electrode through rolling, and includes a controller that can control the thickness and heating temperature of the upper and lower rolls and rolls, and a winding that can unwind and wind the electrode. made up of wealth The rolling process proceeds as the electrode in a roll state passes through the roll press, which is then wound into a roll state to complete the electrode. At this time, it is preferable that the pressing pressure of the press is 5 to 20 ton/cm 2 and the temperature of the roll is 0 to 150°C.

In addition, looking at another example of forming an electrode in the form of an electrode, the composition for a supercapacitor electrode is coated on a metal foil such as a titanium foil, an aluminum foil, or an aluminum etching foil. Alternatively, the composition for supercapacitor electrodes may be made into a sheet state (rubber type) by pushing the composition with a roller, and may be manufactured in an electrode shape by attaching it to a metal foil or a metal current collector. Here, the aluminum etching foil means that the aluminum foil is etched in a concave-convex shape.

Supercapacitor electrode formation

In the supercapacitor electrode forming step ( S130 ), the resultant formed in the form of an electrode is dried to form a supercapacitor electrode.

The composition for supercapacitor electrodes that has been subjected to the press compression process is subjected to a drying process. The drying process is carried out at a temperature of 100 °C to 350 °C, preferably 150 °C to 300 °C. At this time, when the drying temperature is less than 100 ° C., it is not preferable because evaporation of the dispersion medium is difficult, and when drying at a high temperature exceeding 350 ° C., oxidation of the conductive material may occur. Therefore, it is preferable that the drying temperature is at least 100°C or higher and does not exceed 350°C. And, the drying process is preferably carried out at the same temperature as above for 10 minutes to 6 hours. This drying process dries the molded composition for a supercapacitor electrode (evaporating the dispersion medium) and at the same time binds the powder particles to improve the strength of the supercapacitor electrode.

On the other hand, when the electrode is formed by another example of forming an electrode, it is preferably dried at a temperature of 100 to 250 °C, preferably 150 to 200 °C.

The supercapacitor electrode manufactured by the above processes (S110 to S130) has a high capacity and can be usefully applied to a small coin-type supercapacitor.

Electrolyte impregnation

In the electrolyte impregnation step (S140), a supercapacitor electrode is used as an anode and a cathode, a separator is disposed between the anode and the cathode to prevent a short circuit between the anode and the cathode, and the anode and the cathode are immersed in the electrolyte of the supercapacitor.

Here, the electrolyte of the supercapacitor is an electrolyte salt comprising at least one selected _{from MClO 4} , MBF ₄ , MPF ₆ , MTFSI, MFSI and MSO _{4 (where M is Na or K.)} solvents.

The solvent is ethylene carbonate (EC), propylene carbonate (PC), fluoroethylene carbonate (FEC), dimethyl carboenite (DMC), diethyl carbonate (DEC), dimethyl carbonate (EMC), dimethoxyethane (DME), It may include at least one selected from tetraethylene glycol dimethyl ether (TEGDME), diethylene glycol dimethyl ether (DEGDME), and water.

Example

Hereinafter, the configuration and operation of the present invention will be described in more detail through preferred embodiments of the present invention. However, this is presented as a preferred example of the present invention and cannot be construed as limiting the present invention in any sense.

Content not described here will be omitted because it can be technically inferred sufficiently by a person skilled in the art.

1. Manufacture of biocompatible electrode active material

Example 1

Ti(SO ₄ ) ₂ After completely dissolving in distilled water, H ₃ PO ₄ and NH ₃ H ₂ O were added, followed by stirring for 6 hours.

Next, the resultant stirred in a white emulsion state was put into a microwave container, and then microwave treatment was performed for 20 minutes at 400 W and 300 psi using a microwave (MARS, CEM Corp.).

Next, the resultant wave-treated with a mask was stirred in distilled water, washed until pH reached 7, filtered, and dried at 120° C. for 24 hours _{to obtain Na 4} TiPO ₄ (NTP).

_{Next, NaNO 3} : NTP was mixed in 500 ml of distilled water in a weight ratio of 3 : 1 and stirred at 100 ° C., stirred for 2 hours, stirred for 6 hours while heating to 300 ° C., and then using distilled water to pH After neutralization and filtration until 7, the electrode was dried at 120° C. for 24 to prepare an electrode active material composed of a compound having a structure of _{NaTiOPO 4 .}

Example 2

A biocompatible electrode active material was prepared in the same manner as in Example 1, except that microwave treatment was performed for 25 minutes under conditions of 350 W and 250 psi.

Example 3

A biocompatible electrode active material was prepared in the same manner as in Example 1, except that microwave treatment was performed for 25 minutes under conditions of 450 W and 250 psi.

Example 4

A biocompatible electrode active material was prepared in the same manner as in Example 1, except that _{NaNO 3 : NTP was mixed in a weight ratio of 4 : 1.}

Comparative Example 1

A biocompatible electrode active material was prepared in the same manner as in Example 1, except that microwave treatment was performed for 5 minutes under conditions of 200 W and 200 psi, and NaNO _{3 : NTP was mixed in a weight ratio of 1:1.}

2. Cell viability test

Table 1 shows the cell viability test results for the biocompatible electrode active materials prepared according to Examples 1 to 4 and Comparative Example 1.

Test Methods

In vitro cytotoxicity tests were performed using the Cell Counting Kit-8 (CCK-8) assay (CK04-11, Dojindo, Japan) for human fibroblast fibroblast) and monkey kidney fibroblast-like (COS-7) cells. . Dulbecco's Modified Eagle's Medium (DMEM) containing 10% fetal bovine serum (FBS; Gibco, USA) and 1% penicillin-streptomycin (Gibco, USA) at 37°C for both cell types ; Gibco, Lifetechnology Inc., USA) in 37 ℃, 5% CO _{2 It} was cultured in an environment.

To evaluate the cytotoxicity of the material, samples of the type dispersed in deionized water were prepared using a sonicator. Fibroblasts and COS-7 were seeded in 24-well cell culture plates at ^{3.0 × 10 4 cells per well and cultured for 24 hours.} Cells were then _{incubated in NaTiOPO 4} dispersion for 24 h. Cells were washed 3 times with dPBS, and 500 μl of DMEM supplemented with 10% CCK-8 dye was added to each well and incubated for 2 hours. The absorbance of the supernatant was measured at 450 nm using a microplate reader.

[Table 1]

As shown in Table 1, it can be confirmed that the biocompatible electrode active materials prepared according to Examples 1 to 4 satisfy all of the cell viability of 70% or more corresponding to the target value.

On the other hand, the cell viability of the biocompatible electrode active material prepared according to Comparative Example 1 was less than the target value.

In addition, Figure 3 is a graph showing the cell viability test results for the supercapacitor having the biocompatible electrode active material prepared according to Examples 1-2. Here, the cell viability is measured after preparing a supercapacitor using the biocompatible electrode active material prepared according to Examples 1 and 2 as a negative electrode and a positive electrode active material of the supercapacitor, respectively, and storing it at room temperature for 5 days.

As shown in Figure 3, the cell viability test results for the supercapacitor using the biocompatible electrode active material prepared according to Examples 1 and 2 as the negative and positive electrode active materials of the supercapacitor, respectively, showed that the cell viability was 90% or more. can be checked

In the above, the embodiments of the present invention have been mainly described, but various changes or modifications can be made at the level of those skilled in the art to which the present invention pertains. Such changes and modifications can be said to belong to the present invention without departing from the scope of the technical spirit provided by the present invention. Accordingly, the scope of the present invention should be judged by the claims described below.

S10: starting material synthesis step
S20: mixing and bathing step
S30: heating and drying step
S110: Formation step of composition for supercapacitor electrode
S120: Formation step in the form of an electrode
S130: Supercapacitor electrode formation step
S140: electrolyte impregnation step

Claims (14)

As a biocompatible electrode active material comprising a compound having the structure of the following [Formula 1],
The electrode active material is accompanied by an electrochemical reaction in an electrolyte containing Na or K,
The electrolyte _{includes an electrolyte salt comprising at least one selected from MClO 4} , MBF ₄ , MPF ₆ , MTFSI, MFSI and MSO ₄ (where M is Na or K), and a solvent dissolving the electrolyte salt A biocompatible electrode active material, characterized in that.
[Formula 1]: ATiOPO ₄
(Where [A] is Na or K.)
According to claim 1,
By having the structure of the above [Formula 1],
A biocompatible electrode active material, characterized in that it is used as an electrode active material of a supercapacitor through an electrochemical reaction in a body fluid.
According to claim 1,
The electrode active material is
It further comprises at least one carbon material selected from carbon nanotubes, carbon nanofibers, graphene and activated carbon,
A biocompatible electrode active material, characterized in that it can be compounded by mixing with the carbon material.
delete delete According to claim 1,
The solvent is
Ethylene carbonate (EC), propylene carbonate (PC), fluoroethylene carbonate (FEC), dimethyl carboenite (DMC), diethyl carbonate (DEC), dimethyl carbonate (EMC), dimethoxyethane (DME), tetraethylene A biocompatible electrode active material comprising at least one selected from glycol dimethyl ether (tetraethylene glycol dimethyl ether, TEGDME), diethylene glycol dimethyl ether (DEGDME), and water.
(a) synthesizing _{Na 4} TiPO _{4 as a starting material;}
(b) _{mixing the synthesized Na 4} TiPO ₄ with potassium nitrate or sodium nitrate and bathing at 80 to 120° C., followed by stirring; and
(c) the resultant of step (b) is stirred while heating to 250 ~ 350 ℃, neutralized until pH 6.5 ~ 7.5 using distilled water, filtered and dried to obtain a compound having the structure of the following formula (1) obtaining an electrode active material consisting of;
A method for producing a biocompatible electrode active material comprising a.

[Formula 1]: ATiOPO ₄
(Where [A] is Na or K.)
8. The method of claim 7,
The step (a) is,
(a-1) _{after dissolving Ti(SO 4} ) ₂ in distilled water, _{adding H 3} PO ₄ and NH ₃ H ₂ O and stirring for 5 to 7 hours;
(a-2) microwave-treating the stirred resultant into a microwave container; and
(a-3) The microwave-treated product is stirred in distilled water, washed until pH is 6.5 to 7.5, filtered, and dried at 100 to 140° C. for 20 to 30 hours to obtain _{NH 4} TiOPO _{4 .} ;
A method for producing a biocompatible electrode active material comprising a.
9. The method of claim 8,
The microwave treatment is
A method of manufacturing a biocompatible electrode active material, characterized in that it is carried out for 10 to 30 minutes under the conditions of 350 ~ 450W and 250 ~ 350psi.
8. The method of claim 7,
In step (b),
The Na ₄ TiPO ₄ and potassium nitrate or sodium nitrate 1: 2 to 1: A method for producing a biocompatible electrode active material, characterized in that mixed in a weight ratio of 4.
8. The method of claim 7,
In step (c),
the drying
A method for producing a biocompatible electrode active material, characterized in that carried out at 100 ~ 140 ℃ for 20 ~ 30 hours.
The positive electrode and the negative electrode are disposed to be spaced apart from each other, and a separator is disposed between the positive electrode and the negative electrode to prevent a short circuit between the positive electrode and the negative electrode, and the positive electrode and the negative electrode are impregnated with an electrolyte of a supercapacitor,
Each of the positive and negative electrodes includes an electrode active material, a conductive material and a binder,
At least one of the electrode active materials of the positive electrode and the negative electrode consists of a compound having a structure of the following [Formula 1],
At least one of the electrode active materials of the positive electrode and the negative electrode is accompanied by an electrochemical reaction in an electrolyte containing Na or K,
The electrolyte _{includes an electrolyte salt comprising at least one selected from MClO 4} , MBF ₄ , MPF ₆ , MTFSI, MFSI and MSO ₄ (where M is Na or K), and a solvent dissolving the electrolyte salt A supercapacitor having a biocompatible electrode active material, characterized in that
[Formula 1]: ATiOPO ₄
(Where [A] is Na or K.)
delete 13. The method of claim 12,
The solvent is
Ethylene carbonate (EC), propylene carbonate (PC), fluoroethylene carbonate (FEC), dimethyl carboenite (DMC), diethyl carbonate (DEC), dimethyl carbonate (EMC), dimethoxyethane (DME), tetraethylene A supercapacitor having a biocompatible electrode active material, comprising at least one selected from glycol dimethyl ether (tetraethylene glycol dimethyl ether, TEGDME), diethylene glycol dimethyl ether (DEGDME), and water.

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