CN104167298A - Graphene-protein derived carbon supercapcaitor material and preparation method thereof - Google Patents
Graphene-protein derived carbon supercapcaitor material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of a supercapaicotr material, and specifically discloses a graphene-protein derived carbon supercapcaitor material and a preparation method thereof. A solution for a protein to coat grapheme is prepared through interaction between the water-soluble protein and the grapheme; and a pore forming agent is added, drying is performed after uniform mixing, and high-temperature carbonization is carried out, such that the porous graphene-water-soluble-protein derived carbon composite material is prepared. The preparation method is simple, green and mild, energy is reduced, the efficiency is high, the cost is low, and the yield is high. The prepared graphene-protein derived carbon composite material is tight and uniform, is large in specific surface area, is of a multi-tunnel structure, and is good in conductivity. A supercapacitor prepared by use of the material has quite good power multiplying performance and circulating stability, and can also demonstrate an ultrahigh specific capacity in the condition of a large current density, thereby having wide application prospect in such fields as new energy eclectic vehicles, hybrid power vehicles, wind power generation, solar energy generation and the like.
Description
Technical field
The invention belongs to new energy materials technical field, be specifically related to class Graphene-protein derived carbon supercapacitor material and preparation method thereof.
Background technology
The development of ultracapacitor starts from the sixties in 20th century, the rise in the nineties in 20th century due to hybrid-electric car, and it has been subject to paying close attention to widely and starting developing rapidly.Ultracapacitor is a kind of Novel energy storage apparatus between traditional capacitor and rechargeable battery, have power density high, have extended cycle life, can instantaneous large-current the feature such as wide, the safety non-pollution of fast charging and discharging, operating temperature range and researcher's favor extremely both at home and abroad has broad application prospects at the military numerous areas that waits of electric automobile uninterrupted power supply Aero-Space.
According to the storage of electric energy and transformation mechanism, ultracapacitor is divided into double electric layer capacitor (electric double layer capacitors, EDLC) and pseudo capacitance device (be again fake capacitance device, pseudo-capacitors), wherein pseudo capacitance device comprises again metal oxide capacitor and conducting polymer capacitor.And in double electric layer capacitor, material with carbon element is most study, be most widely used, mainly comprise active carbon, mesoporous carbon, carbon nano-tube, Carbide-derived carbons, Graphene etc.The carbon of people to various biogenetic derivations recently, the derived carbon such as such as silk-fibroin, hair, Egg-white derived carbon and leaf, wood chip, pollen, cow dung are studied more deeply.Because heteroatomic doping wherein makes these material with carbon elements have higher electric capacity under low current density, but wherein often capacitance loss is serious under high current density for most materials.
Graphene, has excellent mechanics, calorifics electric property and optical property, is the current known best material of electric conductivity at normal temperatures.In pseudo capacitance device, people, often by compound to Graphene and active material, improve the conductivity of material and then reduce the capacitance loss of material under high current density.But, these complex methods often more complicated or composite effect not satisfactory.
The present invention proposes class Graphene-protein derived carbon supercapacitor material and preparation method thereof.Utilize the interaction of water soluble protein and Graphene to reach the compound of itself and graphene uniform.By simple pore-foaming agent pore carbonization, the final Graphene obtaining-protein derived carbon composite has multiple pore passage structure, high reference area, good material conductivity and excellent ultracapacitor electrical property.Make various biogenic material with carbon elements there is considerable actual application prospect in ultracapacitor field.
Summary of the invention
The object of the invention is to provide a kind of super capacitor material and preparation method thereof, i.e. class Graphene-protein derived carbon supercapacitor material and preparation method thereof.Graphene-protein derived the carbon composite obtaining by the method has multiple pore passage structure, high reference area, good material conductivity and excellent ultracapacitor electrical property.
The present invention is realized by the following technical programs: first water-solubility protein is mixed with graphene oxide, reduction under certain condition, add again pore-foaming agent, be dried, after atmosphere of inert gases carbonization, obtain Graphene-water soluble protein derived carbon composite material of porous.
The preparation method of Graphene-protein derived carbon supercapacitor material provided by the invention, concrete steps are as follows:
(1) first, prepare the aqueous solution of water soluble protein, its mass fraction 0.5 ~ 20%; Prepare graphene oxide, its mass fraction is 0.01% ~ 5%, is of a size of 50 nm ~ 50 μ m; Under stirring at room temperature, above-mentioned two kinds of solution are mixed under the condition of pH=6 ~ 14, both mass ratioes can 1:50 ~ 50:1(preferably both mass ratioes be 1:10 ~ 10:1) scope in regulation and control, stirring, obtains water soluble protein and graphene oxide mixed solution;
(2) then, carry out reduction reaction, reduction reaction can be under strong alkaline condition and reduces, and utilizes reproducibility amino acid reduction on albumen, or adds reducing agent reduction; Reduction reaction temperature is 30 ~ 250 DEG C, after reaction 0.5h ~ 3d. reaction finishes, obtains the stable redox graphene of water soluble protein;
(3) then, in solution obtained above, add pore-foaming agent, stir 0.5h ~ 2h; Be dried processing, drying condition is vacuumize, water the one in the dry and freeze drying of film again;
(4) last, carry out carbonization treatment, carbonization is carried out under the atmosphere of nitrogen or argon gas, and temperature is 500 ~ 900 DEG C, and heating rate is 5 ~ 30 DEG C/min; Carbonization time is 1 ~ 5h;
(5) after carbonization, water respectively, ethanol cleans repeatedly; Under the condition of 30 ~ 50 DEG C of vacuum drying ovens, be dried 3 ~ 8h, obtain Graphene-protein derived carbon composite of porous.
In the present invention, reduction reaction reducing agent used can be but is not limited to the one in hydrazine hydrate, citric acid, hydroiodic acid and hydrobromic acid.
In the present invention, described pore-foaming agent is KOH, NaOH, Na
2cO
3, NaHCO
3, K
2cO
3and KHCO
3one or more components.The mass ratio of pore-foaming agent and compound is 1:10 ~ 10:1, and preferred mass is than being 1:5 ~ 5:1
Graphene-protein derived carbon composite prepared by the present invention, contained element is carbon, nitrogen, oxygen; Specific area is 200 ~ 3500 m
2/ g; Pore-size distribution is 1 ~ 1000 nm; Cyclic voltammetry curve is class rectangle, has the hump that reacts generation due to faraday, and under low current density, the capacity of (0.2 A/g) is 150 ~ 450 F/g; Under high current density, (20 ~ 100 A/g) capacity is greater than 100 F/g.
Graphene-protein derived carbon composite of the prepared porous of the present invention is compound closely evenly, and specific area is large and have multiple pore passage structure, abundant Heteroatom doping, good conductivity.Preparation process is simple, green gentle, efficient energy-saving, and with low cost, productive rate is considerable.Measure the ultracapacitor performance of this material, show the specific capacity (especially under high current density) of superelevation, well high rate performance and cyclical stability.Can be by regulation and control water soluble protein kind, regulate and control the assembling, compound of water soluble protein and graphene sheet layer with the when reduction mode of quality of Graphene, the kind by pore-foaming agent with add controlling of quality pore size distribution and specific area.The conductivity of crystal formation, heteroatomic content and material by the regulation and control such as dry run, carburizing temperature, time Graphene-protein derived carbon composite, and then the important electrical property such as specific capacity, high rate performance and the cyclical stability of the ultracapacitor of regulation and control Graphene-protein derived carbon composite.The ultracapacitor that adopts this type of material to prepare, has good high rate performance, cyclical stability, also can show the specific capacity of superelevation under high current density.There is wide wide application prospect in fields such as New-energy electric vehicle, hybrid vehicle, wind power generation, solar power generations.
Brief description of the drawings
Fig. 1 is Graphene-protein complex atomic force microscope (AFM) photo that embodiment 1 prepares.
Fig. 2 is Graphene-protein derived carbon composite stereoscan photograph that embodiment 1 prepares.
Fig. 3 is Graphene-protein derived carbon composite stereoscan photograph that embodiment 1 prepares.
Fig. 4 is the cyclic voltammetry curve of Graphene-protein derived carbon composite of preparing of embodiment 1.
Fig. 5 is the cyclical stability test curve of Graphene-protein derived carbon composite of preparing of embodiment 1.
Embodiment
Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention, and any simple modification, equivalent variations and modification that every foundation technical spirit of the present invention is done following instance, all still belong in the scope of technical solution of the present invention.
Raw material in following examples is commercial goods.
embodiment 1
1. prepare the aqueous solution of mulberry silk albumen, mass fraction 4%.Prepare graphene oxide, its mass fraction is 0.4%, is of a size of 200 nm.
2. under stirring at room temperature, above-mentioned two kinds of solution are mixed under the condition of pH=8, both mix with volume ratio 1:1, obtain mulberry silk albumen and graphene oxide mixed solution.
3. add natrium citricum reduction, reduction temperature is 100 DEG C, after reaction 3h. reaction finishes, obtains mulberry silk albumen-redox graphene solution.Figure mono-is the atomic force microscope picture of composite solution for this reason, has shown that mulberry silk albumen is being wound around redox graphene and is stoping its large stretch of gathering.
4. in composite solution obtained above, add NaOH, admittedly containing mass ratio with composite solution is 1:1, stirs 0.5h, vacuumize under room temperature.
5. by above-mentioned dried compound carbonization.Under nitrogen atmosphere, temperature is 800 DEG C, and heating rate is 10 DEG C/min.Carbonization time is 3h.Difference water after carbonization, ethanol cleans repeatedly.Under the condition of 30 DEG C of vacuum drying ovens, dry 8h, obtains the protein derived carbon composite of Graphene-mulberry silk.
6. the protein derived carbon composite of the Graphene-mulberry silk of pair gained carries out ESEM, transmission electron microscope observing, on the loose porous and lamella of this material, distributing a large amount of mesoporous/micropore.As Fig. 2, shown in 3.
7. the protein derived carbon composite of the Graphene-mulberry silk of the porous of pair gained carries out the analysis of X-ray powder diffraction, and this material is the graphited carbon of part.By specific area and porosity, it is tested, this material specific area is 1600 m
2/ g; Pore-size distribution is 1 ~ 10 nm.
8. taking the protein derived carbon composite of Graphene-mulberry silk of porous as active material, acetylene black is conductive agent, polytetrafluoroethylene is binding agent, the ratio that is 80:10:10 in mass ratio active material, conductive agent and binding agent is distributed in isopropyl alcohol, bar film, be 30 Mpa lower sheetings to nickel foam upper 30 second at pressure, make electrode of super capacitor.
9. using platinized platinum as to electrode, saturated calomel electrode is reference electrode, and the KOH solution of 6M is electrolyte, carries out cyclic voltammetry, and its cyclic voltammetry curve shows as rectangle, as shown in Figure 4.Its electrochemical reversibility is higher, still can keep higher capacity under high sweep speed.It is carried out to constant current charge-discharge test, and this material has higher specific capacity, and has good cyclical stability.
embodiment 2
1. prepare the aqueous solution of mulberry silk albumen, mass fraction 10%.Prepare graphene oxide, its mass fraction is 1%, is of a size of 200 nm.
2. under stirring at room temperature, above-mentioned two kinds of solution are mixed under the condition of pH=8, both mix with volume ratio 1:2, obtain mulberry silk albumen and graphene oxide mixed solution.
3. add hydrazine hydrate reduction, reduction temperature is 80 DEG C, after reaction 6h. reaction finishes, obtains mulberry silk albumen-redox graphene solution.
4. in composite solution obtained above, add KOH, admittedly containing mass ratio with composite solution is 2:1, stirs 0.5h, freeze-drying.
5. by above-mentioned dried compound carbonization.Under nitrogen atmosphere, temperature is 700 DEG C, and heating rate is 10 DEG C/min.Carbonization time is 3h.Difference water after carbonization, ethanol cleans repeatedly.Under the condition of 30 DEG C of vacuum drying ovens, be dried 8h, obtain the protein derived carbon composite of Graphene-mulberry silk of porous.
6. the protein derived carbon composite of the Graphene-mulberry silk of pair gained carries out scanning electron microscopic observation, and this material is loose porous.By transmission electron microscope also can be observed in sheet of material, distributing a large amount of mesoporous/micropore.The protein derived carbon composite of the Graphene-mulberry silk of gained is carried out to the analysis of X-ray powder diffraction, and this material is the graphited carbon of part.
7. taking the protein derived carbon composite of Graphene-mulberry silk of porous as active material, acetylene black is conductive agent, polytetrafluoroethylene is binding agent, the ratio that is 80:10:10 in mass ratio active material, conductive agent and binding agent is distributed in isopropyl alcohol, bar film, be 30 Mpa lower sheetings to nickel foam upper 30 second at pressure, make electrode of super capacitor.
8. using platinized platinum as to electrode, saturated calomel electrode is reference electrode, and the KOH solution of 6M is electrolyte, carries out cyclic voltammetry, and its cyclic voltammetry curve shows as rectangle.Its electrochemical reversibility is higher, still can keep higher capacity under high sweep speed.It is carried out to constant current charge-discharge test, and this material has higher specific capacity, and has good cyclical stability.Under the current density of 2 A/g, capacity can reach 180 F/g.Under this current density, carry out charge and discharge cycles 2000 and enclose, without obvious capacity attenuation.As shown in Figure 5.
embodiment 3
1. prepare the aqueous solution of mulberry silk albumen, mass fraction 6%.Prepare graphene oxide, its mass fraction is 0.6%, is of a size of 200 nm.
2. under stirring at room temperature, above-mentioned two kinds of solution are mixed under the condition of pH=8, both mix with volume ratio 1:10, obtain mulberry silk albumen and graphene oxide mixed solution.
3. in composite solution obtained above, add NaOH, admittedly containing mass ratio with composite solution is 5:1.Be at 80 DEG C, to carry out reduction reaction in temperature, after reaction 24h. reaction finishes, obtain mulberry silk albumen-redox graphene solution.
4. by above-mentioned dried compound carbonization.Under nitrogen atmosphere, temperature is 700 DEG C, and heating rate is 10 DEG C/min.Carbonization time is 3h.Difference water after carbonization, ethanol cleans repeatedly.Under the condition of 30 DEG C of vacuum drying ovens, be dried 8h, obtain the protein derived carbon composite of Graphene-mulberry silk of porous.
5. the protein derived carbon composite of the Graphene-mulberry silk of pair gained carries out ESEM, transmission electron microscope observing, on the loose porous and lamella of this material, distributing a large amount of mesoporous/micropore.The protein derived carbon composite of the Graphene-mulberry silk of gained is carried out to the analysis of X-ray powder diffraction, and this material is the graphited carbon of part.
6. taking the protein derived carbon composite of Graphene-mulberry silk of porous as active material, acetylene black is conductive agent, polytetrafluoroethylene is binding agent, the ratio that is 80:10:10 in mass ratio active material, conductive agent and binding agent is distributed in isopropyl alcohol, bar film, be 30 Mpa lower sheetings to nickel foam upper 30 second at pressure, make electrode of super capacitor.
7. using platinized platinum as to electrode, saturated calomel electrode is reference electrode, and the KOH solution of 6M is electrolyte, carries out cyclic voltammetry, and its cyclic voltammetry curve shows as the rectangle of standard, and electrochemical reversibility is higher.It is carried out to constant current charge-discharge test, and under the current density of 0.5 A/g, capacity is 150 F/g.
embodiment 4
1. prepare aqueous gelatin solution, mass fraction is 2%.Prepare graphene oxide, its mass fraction is 0.5%, is of a size of 200 nm.
2. at 50 DEG C of water-baths, above-mentioned two kinds of solution are mixed under the condition of pH=8, both mix with volume ratio 1:1, obtain gelatin and graphene oxide mixed solution.
3. add hydrazine hydrate reduction, reduction temperature is 100 DEG C, after reaction 3h. reaction finishes, obtains gelatin-redox graphene solution.
4. in composite solution obtained above, add NaOH, admittedly containing mass ratio with composite solution is 1:5.Stir 0.5h, freeze-drying.
5. by the compound carbonization of above-mentioned freeze-drying.Under nitrogen atmosphere, temperature is 700 DEG C, and heating rate is 10 DEG C/min.Carbonization time is 3h.Difference water after carbonization, ethanol cleans repeatedly.Under the condition of 30 DEG C of vacuum drying ovens, dry 8h, obtains Graphene-gelatin derived carbon composite material.
6. this Graphene-gelatin derived carbon composite material is loose porous, and it is carried out to the analysis of X-ray powder diffraction, and this material is the graphited carbon of part.
7. taking Graphene-gelatin derived carbon composite material of porous as active material, acetylene black is conductive agent, polytetrafluoroethylene is binding agent, the ratio that is 80:10:10 in mass ratio active material, conductive agent and binding agent is distributed in isopropyl alcohol, bar film, be 30 Mpa lower sheetings to nickel foam upper 30 second at pressure, make electrode of super capacitor.
8. using platinized platinum as to electrode, saturated calomel electrode is reference electrode, and the KOH solution of 6M is electrolyte, carries out cyclic voltammetry, and its cyclic voltammetry curve shows as rectangle.It is carried out to constant current charge-discharge test, and under the current density of 0.2 A/g, its capacity can reach 290 F/g.
embodiment 5
1. prepare aqueous gelatin solution, mass fraction is 5%.Prepare graphene oxide, its mass fraction is 0.5%, is of a size of 200 nm.
2. at 50 DEG C of water-baths, above-mentioned two kinds of solution are mixed under the condition of pH=8, both mix with volume ratio 2:1, obtain gelatin and graphene oxide mixed solution.
3. add natrium citricum reduction, reduction temperature is 100 DEG C, after reaction 3h. reaction finishes, obtains gelatin-redox graphene solution.
4. in composite solution obtained above, add KOH, admittedly containing mass ratio with composite solution is 1:1., freeze-drying.
5. by the compound carbonization of above-mentioned freeze-drying.Under nitrogen atmosphere, temperature is 900 DEG C, and heating rate is 10 DEG C/min.Carbonization time is 3h.Difference water after carbonization, ethanol cleans repeatedly.Under the condition of 30 DEG C of vacuum drying ovens, dry 8h, obtains Graphene-gelatin derived carbon composite material.
6. this Graphene-gelatin derived carbon composite material is loose porous, and it is carried out to the analysis of X-ray powder diffraction, and this material is the graphited carbon of part.
7. taking Graphene-gelatin derived carbon composite material of porous as active material, acetylene black is conductive agent, polytetrafluoroethylene is binding agent, the ratio that is 80:10:10 in mass ratio active material, conductive agent and binding agent is distributed in isopropyl alcohol, bar film, be 30 Mpa lower sheetings to nickel foam upper 30 second at pressure, make electrode of super capacitor.
8. using platinized platinum as to electrode, saturated calomel electrode is reference electrode, and the KOH solution of 6M is electrolyte, carries out cyclic voltammetry, and its cyclic voltammetry curve shows as rectangle.It is carried out to constant current charge-discharge test, and under the current density of 2 A/g, capacity is 172 F/g.
Claims (4)
1. the preparation method of class Graphene-protein derived carbon supercapacitor material, is characterized in that, concrete steps are as follows:
(1) first, prepare the aqueous solution of water soluble protein, its mass fraction 0.5 ~ 20%; Prepare graphene oxide, its mass fraction is 0.01% ~ 5%, is of a size of 50 nm ~ 50 μ m; Under stirring at room temperature, above-mentioned two kinds of solution are mixed under the condition of pH=6 ~ 14, both mass ratioes can regulate and control in the scope of 1:50 ~ 50:1, stir, and obtain water soluble protein and graphene oxide mixed solution;
(2) then, carry out reduction reaction, reduction reaction temperature is 30 ~ 250 DEG C, after reaction 0.5h ~ 3d. reaction finishes, obtains the stable redox graphene of water soluble protein;
(3) then, in solution obtained above, add pore-foaming agent, stir 0.5h ~ 2h; Be dried processing, drying condition is vacuumize, water the one in the dry and freeze drying of film again;
(4) last, carry out carbonization treatment, carbonization is carried out under the atmosphere of nitrogen or argon gas, and temperature is 500 ~ 900 DEG C, and heating rate is 5 ~ 30 DEG C/min; Carbonization time is 1 ~ 5h;
(5) after carbonization, water respectively, ethanol cleans repeatedly; Under the condition of 30 ~ 50 DEG C of vacuum drying ovens, be dried 3 ~ 8h, obtain Graphene-protein derived carbon composite of porous.
2. preparation method according to claim 1, is characterized in that reduction reaction reducing agent used is the one in hydrazine hydrate, citric acid, hydroiodic acid and hydrobromic acid.
3. preparation method according to claim 1, is characterized in that described pore-foaming agent is KOH, NaOH, Na
2cO
3, NaHCO
3, K
2cO
3and KHCO
3in one, or wherein multiple; The mass ratio of pore-foaming agent and compound is 1:10 ~ 10:1.
4. Graphene-protein derived carbon supercapacitor material that the preparation method as described in one of claim 1-3 prepares, contained element is carbon, nitrogen, oxygen; Specific area is 200 ~ 3500 m
2/ g; Pore-size distribution is 1 ~ 1000 nm; Cyclic voltammetry curve is class rectangle, has the hump that reacts generation due to faraday, and the capacity under 0.2 A/g low current density is 150 ~ 450 F/g; Under 20 ~ 100 A/g high current densities, capacity is greater than 100 F/g.
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| CN105551829A (en) * | 2015-12-16 | 2016-05-04 | 天津工业大学 | Sandwich structured porous carbon/graphene composite material and application in supercapacitor |
| CN105810442A (en) * | 2016-03-16 | 2016-07-27 | 长春工业大学 | Fabrication method of g-C3N4 reinforced solar cell |
| CN105869903A (en) * | 2016-05-25 | 2016-08-17 | 全球能源互联网研究院 | Preparation method of graphene |
| CN108517238A (en) * | 2018-04-04 | 2018-09-11 | 中国科学院宁波材料技术与工程研究所 | Protein modification redox graphene water lubrication additive, its preparation method and application |
| KR102450040B1 (en) * | 2022-02-04 | 2022-10-05 | (주)마중물 | Manufacturing method of food packaging container with graphene |
| KR102455672B1 (en) * | 2022-02-04 | 2022-10-19 | (주)마중물 | Method for manufacturing food packaging material using pellet with graphene |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105551829A (en) * | 2015-12-16 | 2016-05-04 | 天津工业大学 | Sandwich structured porous carbon/graphene composite material and application in supercapacitor |
| CN105810442A (en) * | 2016-03-16 | 2016-07-27 | 长春工业大学 | Fabrication method of g-C3N4 reinforced solar cell |
| CN105869903A (en) * | 2016-05-25 | 2016-08-17 | 全球能源互联网研究院 | Preparation method of graphene |
| CN105869903B (en) * | 2016-05-25 | 2021-03-02 | 全球能源互联网研究院 | Graphene preparation method |
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| CN108517238B (en) * | 2018-04-04 | 2021-04-02 | 中国科学院宁波材料技术与工程研究所 | Protein-modified reduced graphene oxide water lubricating additive, and preparation method and application thereof |
| KR102450040B1 (en) * | 2022-02-04 | 2022-10-05 | (주)마중물 | Manufacturing method of food packaging container with graphene |
| KR102455672B1 (en) * | 2022-02-04 | 2022-10-19 | (주)마중물 | Method for manufacturing food packaging material using pellet with graphene |
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Application publication date: 20141126 |