Sulfur, nitrogen and transition metal doped graphene, preparation method and application thereof

A transition metal and graphene technology, applied in the field of electrochemistry, can solve the problems of relatively high corrosion resistance of equipment and environmental pollution, and achieve the effects of excellent catalytic performance, environmental friendliness, and simple preparation method.

Inactive Publication Date: 2017-07-18
SOUTH CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the heteroatom-doped graphene in the above two patents often needs to use gaseous heteroatom sources (involving pungent and corrosive gases such as ammonia and sulfur dioxide) and flammable gases such as methane and hydrogen during the preparation process. Explosive gas, easy to cause pollution to the environment, and requires relatively high corrosion resistance of equipment

Method used

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  • Sulfur, nitrogen and transition metal doped graphene, preparation method and application thereof
  • Sulfur, nitrogen and transition metal doped graphene, preparation method and application thereof

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[0025] The preparation method of above-mentioned sulfur, nitrogen, transition metal doped graphene comprises the following steps:

[0026] 1) Add graphene or graphite oxide, transition metal compound, nitrogen-containing compound and sulfur-containing compound into the solvent, mix well, then dry and grind to obtain solid powder;

[0027] 2) Place the solid powder in step 1) in a vacuum or an inert gas, raise the temperature to 350-1200°C at a heating rate of 3-10°C / min, keep it warm for 0.5-6h, and then lower the temperature at a rate of 3-10°C / min Cool down to room temperature to obtain sulfur, nitrogen, and transition metal doped graphene.

[0028] Preferably, the mass ratio of graphene or graphite oxide, transition metal compound, nitrogen-containing compound, and sulfur-containing compound in step 1) is 1:0.1-2:0.1-5:0.1-5.

[0029] Preferably, the mass volume ratio of the graphene or graphite oxide and the solvent in step 1) is 1 g: 100-1000 mL.

[0030] Preferably, th...

Embodiment 1

[0038] Weigh 0.3g of graphene, 0.3g of cobalt acetate, 0.3g of phthalocyanine and 0.3g of dibenzyl disulfide into 40mL of ethanol solution. After drying for 2 hours in a vacuum oven, dry it in a vacuum oven for 10 hours; grind the obtained product into powder, put it into a porcelain boat and put it into a tube furnace for pyrolysis, raise the temperature to 900 ° C at a heating rate of 5 min / ° C in an argon atmosphere, and Keep it warm for 1 hour, and then cool down to room temperature at a cooling rate of 5°C / min to obtain cobalt-sulfur-nitrogen-doped graphene.

Embodiment 2

[0040] Weigh 0.1g of graphene, 0.2g of cobalt acetate, 0.3g of phthalocyanine and 0.3g of dibenzyl disulfide, add them into 40mL of isopropanol solution, stir and mix evenly, ultrasonicate for 3h, then evaporate the ethanol solution to dryness, After drying in an air oven for 2 hours, dry in a vacuum oven for 10 hours; grind the resulting product into powder, put it into a porcelain boat and put it into a tube furnace for pyrolysis, and heat up to 500°C at a heating rate of 3min / °C in an argon atmosphere , and keep it warm for 5h, and then cool down to room temperature at a cooling rate of 3°C / min to obtain cobalt-sulfur-nitrogen-doped graphene.

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Abstract

The invention discloses a sulfur, nitrogen and transition metal doped graphene, a preparation method and an application thereof. Sulfur and nitrogen are doped and transition metal is loaded in the doped graphene. The preparation method of the doped graphene comprises the following steps: 1) adding graphene or graphite oxide, transition metal compound, nitrogen-containing compound and sulfur-containing compound into a solvent, fully and uniformly mixing, drying and grinding, thereby acquiring solid powder; and 2) placing the solid powder acquired in step 1) into vacuum or inert gas, increasing the temperature to 350-1200 DEG C at the heating rate of 3-10 DEG C/min, keeping the temperature for 0.5-6 hours and then reducing the temperature to room temperature at the cooling rate of 3-10 DEG C/min. The sulfur, nitrogen and transition metal doped graphene disclosed by the invention has an excellent catalytic performance; the preparation method is simple; the adopted raw materials are all nontoxic; the sulfur, nitrogen and transition metal doped graphene is environment-friendly, is easily popularized and is widely applied to the fields of primary lithium battery, lithium ion battery, fuel cell, solar cell, super-capacitor, and the like.

Description

technical field [0001] The invention relates to a sulfur, nitrogen and transition metal doped graphene and a preparation method and application thereof, belonging to the technical field of electrochemistry. Background technique [0002] Graphene, also known as monoatomic layer graphite, is a honeycomb planar film formed by sp2 hybridization of carbon atoms. It has a large specific surface area, good flexibility, and excellent electrical and thermal conductivity. It is widely used in electronics, sensors, and supercapacitors. And batteries and other fields have great application prospects. Experiments have shown that the doping of heteroatoms such as nitrogen, boron, sulfur, phosphorus and halogen elements can further adjust and change the electrical properties and chemical stability of graphene. Patent CN102738476A discloses a nitrogen-doped graphene-loaded transition metal cathode, which is used in a sodium borohydride fuel cell, and the power generation performance of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/194H01M4/583H01M4/62H01G11/32
CPCC01P2006/40H01G11/32H01M4/583H01M4/625Y02E60/10Y02E60/13
Inventor 袁中直钟秀文赖彩婷
Owner SOUTH CHINA NORMAL UNIVERSITY
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