CN104192830A - Preparing method of nitrogen-sulfur co-doped graphene by hydrothermal method - Google Patents
Preparing method of nitrogen-sulfur co-doped graphene by hydrothermal method Download PDFInfo
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- CN104192830A CN104192830A CN201410214966.5A CN201410214966A CN104192830A CN 104192830 A CN104192830 A CN 104192830A CN 201410214966 A CN201410214966 A CN 201410214966A CN 104192830 A CN104192830 A CN 104192830A
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Abstract
The invention discloses a preparing method of nitrogen-sulfur co-doped graphene by a hydrothermal method. According to the method, graphene oxide and thiourea are adopted as raw materials, and a cathode catalyst in replace of commercial Pt/C catalysts for fuel cells and metal-air batteries is prepared through a low-temperature one-step hydrothermal reaction. The preparing method is simple and easy in operation. Post-treatment washing and post-treatment drying are convenient. The preparing method can be performed at a low temperature and saves a large amount of energy when compared with high-temperature annealing. The reaction time is short so that products can be obtained more rapidly and the production efficiency is increased when the preparing method is compared with biological reduction methods. Production equipment is simple, and only one industrial reactor is needed, so that the production cost is largely reduced. The preparing method is characterized by simple steps, high production efficiency, low cost, easy byproduct treatment and no pollution to the environment.
Description
Technical field
The present invention relates generally to Graphene preparation and doping vario-property technology, and application in fuel cell and metal-air battery cathod catalyst.
Background technology
Enter 21 century, energy problem becomes increasingly conspicuous, and becomes the significant problem of restriction growth of the national economic.Devoting Major Efforts To Developing, the green energy resource of expanding novel sustainability and storage thereof, switch technology are the only ways addressing this problem.
Fuel cell is a kind of novel energy conversion device, it can be converted into electric energy by the chemical energy of fuel, and energy efficiency is very high, and produces hardly obnoxious flavour in reaction process, therefore, fuel cell is acknowledged as one of 21 century novel clean, efficient electrochemical energy.Fuel cell is mainly made up of this four part of negative electrode, anode, ionogen and external circuit, and anode is hydrogen electrode, and negative electrode is oxygen electrode, and the process essence of whole Conversion of energy is exactly redox reaction.
Fuel cell has huge market potential, very likely becomes one of main energy sources of Future Society.But want to realize fuel cell large-scale commercial application, also have many difficult problems to be badly in need of breaking through, wherein most important, distinct issues are to find suitable cathod catalyst.At present, the cathod catalyst of business is Pt/C catalyzer, but the reserves of Pt are limited, expensive, in reaction process, be easily subject to the impact of methyl alcohol and intermediate product CO and the poisoning catalytic activity that loses, therefore business Pt/C is not suitable for doing the cathod catalyst of fuel cell simultaneously.
Graphene is a kind of carbon atom SP
2the monolayer carbon nano material of hydridization, there is good conductivity and huge specific surface area, this makes Graphene aspect heavy-duty battery and electrode material for super capacitor, have huge application potential, a large amount of Graphenes that studies have shown that Heteroatom doping can improve the catalytic activity of hydrogen reduction simultaneously, the researchist who wears seminar at dawn finds that the nitrogen co-doped Graphene of boron has excellent hydrogen reduction performance, toxin immunity and stability (Angew. Chem., Int. Ed., 2012, 51, 4209 – 4212), the Qiao Shi chapter researchist of seminar finds that nitrogen sulphur codoped Graphene has outstanding hydrogen reduction performance (Angew. Chem. equally, Int. Ed., 2012, 51, 11496 – 11500), these catalyzer are all expected to replace business Pt/C becomes fuel battery cathod catalyst.Domestic researchist has also done a large amount of research work to this, and has applied for Patents.Professor Wang Haihui of South China Science & Engineering University application about nitrogen sulphur codoped Graphene patent (publication number CN 103172057), adopt method calcined oxide Graphene and the nitrogen sulphur source of high temperature annealing, the method high energy consumption, produces poisonous tail gas difficult; Professor Wang Shuai of the Central China University of Science and Technology has also applied for about nitrogen sulphur codoped Graphene patent (publication number CN 103255177 A), adopt sulphate reducing bacteria bacteria suspension redox graphene, the method requirement condition harshness (isolated air), long reaction time, preparation process is loaded down with trivial details, is not suitable for equally scale operation.
Summary of the invention
Goal of the invention: the problem and the defect that exist for above-mentioned prior art, the invention provides a kind of hydrothermal method and prepare the method for nitrogen sulphur codoped Graphene, using graphene oxide and thiocarbamide as raw material, prepare through low temperature one step hydro-thermal reaction the method that fuel cell and metal-air battery cathod catalyst replace business Pt/C catalyzer.
Summary of the invention: for solving above-mentioned technical problem, the technical solution adopted in the present invention is: a kind of hydrothermal method is prepared the method for nitrogen sulphur codoped Graphene, comprises the following steps:
(1) Hummers legal system is for graphite oxide;
(2) take the graphite oxide preparing in step (1) and be dissolved in the ultrapure water of 30ml, and ultrasonic 1～2h obtains graphite oxide aqueous solution; Then take thiocarbamide and be dissolved in graphite oxide aqueous solution, then fully stir until thiocarbamide all dissolves;
(3) solution step (2) being obtained packs in hydrothermal reaction kettle, and reacts 10～18h at 150～200 DEG C;
(4) reaction finishes rear cool to room temperature, obtains cylindrical sample, and repeatedly cleans with ultrapure water and dehydrated alcohol, and at 60 ± 5 DEG C, vacuum-drying obtains nitrogen sulphur codoped Graphene.
The weight ratio of described graphite oxide and thiocarbamide is 1:8～12.
Beneficial effect: compared with prior art, the present invention has the following advantages: be only a step hydro-thermal reaction, simple to operation, aftertreatment washing and drying is very convenient; Low temperature, compares high temperature annealing, has saved a large amount of energy; Reaction times is short, compares biological reducing method, can obtain faster product, has improved production efficiency; Production unit is simple, only needs one of industrial reaction still, and production cost reduces greatly; Step is simple, and production efficiency is high, and cost is low, and by product is easily processed, free from environmental pollution.
Brief description of the drawings
Fig. 1 is the method process flow diagram that hydrothermal method of the present invention is prepared nitrogen sulphur codoped Graphene.
embodiment:
Further set forth the present invention below in conjunction with the drawings and specific embodiments.
1. material preparation
(1) raw material: 30g graphene oxide, 300g thiocarbamide (graphene oxide and thiocarbamide mass ratio are that 1:10 sulphur nitrogen-atoms is than being 1:2), 30L ultrapure water
(2) plant and instrument: stirrer, ultrasonic apparatus, 50L high pressure stainless steel cauldron, vacuum drying oven
(3) experimental procedure:
1. the graphene oxide of 30g is dissolved in the ultrapure water of 30L, stirs the sufficiently long time, more ultrasonic to fully dissolving, then add the thiocarbamide of 300g, be stirred well to whole dissolvings;
2. solution step being obtained in is 1. put into the hydrothermal reaction kettle of 50L, adjusts the temperature to 150-200 DEG C, maintains 12h;
3. treat that hydrothermal reaction kettle naturally cools to room temperature, take out the product that hydro-thermal obtains, repeatedly clean with ultrapure water and dehydrated alcohol, 60 DEG C of 24h of vacuum-drying obtain nitrogen sulphur codoped Graphene.
2. product application
(1) fuel cell and metal-air battery cathod catalyst
Hydrogen reduction performance (ORR) test:
1. take the ethanol solution of 2mg nitrogen sulphur codoped Graphene configuration 2mg/mL, ultrasonic, add 50uL naphthols, more ultrasonic;
2. use respectively the Al of 0.3um and 50nm
2o
3the each 15min of powder polishing glass-carbon electrode, with the special Al of RRDE
2o
3powder polishing rotating disk electrode 15min, the electrode that ultrasonic cleaning is polished, dries;
3. the solution 5uL getting in step 1 drips respectively in glass-carbon electrode and rotating disk electrode, seasoning
4. survey nitrogen sulphur codoped Graphene life-span (i-t curve, constant potential-0.25V, 40000s, 1600rpm, 0.1M KOH) and methanol tolerance oxidation (1600rpm, 0.1M KOH, 3M methyl alcohol) performance with Shanghai occasion China electrochemical workstation CHI760E, carry out LSV test (1600rpm, 0.1M KOH, sweep fast 10mV/s, potential region-1.2-0V) with rotating disk electrode RRDE-3A
Experimental result and conclusion: nitrogen sulphur codoped Graphene has good hydrogen reduction performance, the business of the comparing platinum carbon catalyst life-span is more lasting and be difficult for poisoningly, is a kind of catalyzer that very likely replaces business platinum charcoal of applicable scale operation.
(2) electrode material for super capacitor
Cyclic voltammetric (CV) test, constant current charge-discharge (CD) test:
1. take the ethanol solution of 2mg nitrogen sulphur codoped Graphene configuration 2mg/mL, ultrasonic, add 50uL naphthols, more ultrasonic;
2. use respectively the Al of 0.3um and 50nm
2o
3the each 15min of powder polishing glass-carbon electrode, ultrasonic cleaning, dries;
3. get the solution 5uL of step in 1. and drip on glass-carbon electrode, seasoning;
4. survey nitrogen sulphur codoped Graphene CV, CD (6M KOH) test with Shanghai occasion China electrochemical workstation CHI760E.
Experimental result and conclusion: nitrogen sulphur codoped Graphene has good capacitive property, is suitable for making electrode material for super capacitor.
Claims (2)
1. hydrothermal method is prepared a method for nitrogen sulphur codoped Graphene, comprises the following steps:
(1) Hummers legal system is for graphite oxide;
(2) take the graphite oxide preparing in step (1) and be dissolved in the ultrapure water of 30ml, and ultrasonic 1～2h obtains graphite oxide aqueous solution; Then take thiocarbamide and be dissolved in graphite oxide aqueous solution, then fully stir until thiocarbamide all dissolves;
(3) solution step (2) being obtained packs in hydrothermal reaction kettle, and reacts 10～18h at 150～200 DEG C;
(4) reaction is cooled to room temperature after finishing, and obtains cylindrical sample, and repeatedly cleans with ultrapure water and dehydrated alcohol, and at 60 ± 5 DEG C, vacuum-drying obtains nitrogen sulphur codoped Graphene.
2. hydrothermal method is prepared the method for nitrogen sulphur codoped Graphene according to claim 1, it is characterized in that: the weight ratio of described graphite oxide and thiocarbamide is 1:8～12.
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