CN104240792A - Composite material of high-nitrogen-doped grapheme and ultrathin MoSe2 nanosheets and preparation method of composite material - Google Patents

Composite material of high-nitrogen-doped grapheme and ultrathin MoSe2 nanosheets and preparation method of composite material Download PDF

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CN104240792A
CN104240792A CN201410391036.7A CN201410391036A CN104240792A CN 104240792 A CN104240792 A CN 104240792A CN 201410391036 A CN201410391036 A CN 201410391036A CN 104240792 A CN104240792 A CN 104240792A
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composite material
graphene
ultra
mose
nitrogen
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CN104240792B (en
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毕恩兵
陈汉
韩礼元
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Shanghai Jiaotong University
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Abstract

The invention provides a composite material of high-nitrogen-doped grapheme and ultrathin MoSe2 nanosheets and a preparation method of the composite material. According to the method, after a molybdenum source, a selenium source and low-nitrogen-doped grapheme which are dissolved in water and ethylene glycol are sufficiently mixed, solvent thermal reaction is conducted under the effect of ethidene diamine serving as an active agent, the ultrathin MoSe2 nanosheets are made to grow on the grapheme evenly, meanwhile, the low-nitrogen-doped grapheme is doped deeply, and finally the composite material of the high-nitrogen-doped grapheme and the ultrathin MoSe2 nanosheets is obtained. The high-nitrogen-doped grapheme/molybdenum selenide nanosheets synthesized through the method have the excellent performances of high conductivity, high catalysis and the like at the same time, and can be widely applied to photocatalysis, chemical catalysis, electrodes of solar cells, electrodes of other new energy batteries and electrode materials of super-capacitors.

Description

High nitrogen doped Graphene and ultra-thin MoSe 2composite material of nanometer sheet and preparation method thereof
Technical field
What the present invention relates to is a kind of composite material and preparation thereof of technical field of nanometer material preparation, specifically a kind of high nitrogen doped Graphene and ultra-thin MoSe 2composite material of nanometer sheet and preparation method thereof.
Background technology
Transition Metal Sulfur, selenides MX 2(M=Mo, W, Nb, Ta; X=S, Se) cause researcher's extensive concern because it has the layer structure similar to Graphene.This kind of material with the performance of its excellence, as catalytic performance, magnetic, semiconductor property etc., and for fields such as photoelectricity, catalysis, superconductions.Except MoS 2outward, MoSe 2also be a kind of transition metal two-dimensional layer material, there is the lamellar structure being similar to graphite, layer between Mo atom and Se atom with covalent bonds, interlayer then connects with Van der Waals force, be easy between layers peel off, this causes its electric conductivity not good, and this is also limit the major reason that its performance improves further.Current about MoSe in addition 2report actually rare, mainly due to synthesis MoSe 2comparatively complicated, present stage synthesis MoSe 2method mainly comprise solid-phase sintering, electrosynthesis, thermal decomposition method, laser solution method etc.But above-mentioned synthesis MoSe 2method all comprise complicated process control, add the production cost of material.
This theory of premium properties of independent material can be concentrated according to nano composite material, for the performance and application of nano material, there is material impact by the structure of appropriate design material.Therefore, for improving ultra-thin MoSe 2the chemical property of nanometer sheet, utilizes and has high-specific surface area, good electric conductivity, the Graphene of superpower mechanical property, preparation nano composite material, the cooperative effect of both utilizations, possess conductive catalytic performance simultaneously, electronic device, new forms of energy electrode material and catalysis material can be widely used in.But the catalysis of common graphene oxide and electric conductivity are not very high, main cause is containing a large amount of defect and oxy radical, hinders the transmission of electronics.Graphene is carried out functionalization to contribute to improving its chemical property, as excellent chemical property can be made it have by N doping.Therefore, the method for solvent heat growth in situ this method is adopted to prepare high nitrogen doped Graphene and ultra-thin MoSe 2nanosheet composite material, for it provides a kind of effective method in the application in the fields such as photocatalysis, solar cell and ultracapacitor.
Through finding the retrieval of prior art, Wang Zhen is in " synthesis of class Graphene MoS2/ graphene composite nano material and the research of electrochemical lithium storage performance thereof " (Zhejiang University, chemistry, 2013, Master's thesis) in disclose a kind of method adopting cationic surfactant to assist, preparation class Graphene (Graphene ?Like, GL) transition metal dichalcogenide MoS 2/ graphene composite nano material, inquires into its growth mechanism and studies its electrochemistry as cathode material of lithium-ion power battery storage lithium performance.By the assistance of softex kw (CTAB), simple liquid phase synthesizing method is utilized to prepare individual layer MoS 2with the composite material of Graphene.
But defect and the deficiency of above-mentioned technology are: (1), in this type of nano composite material, for the further functionalization of Graphene, as heteroatom doping, research is little relatively; (2) expose active site (Active Edge Sites) by surfactant, correlative study is not; (3) in addition, compared to MoS 2, for MoSe 2research considerably less, the particularly high-quality MoSe of liquid phase synthesis 2this is also a larger difficulty.
Summary of the invention
The present invention is directed to prior art above shortcomings, propose a kind of high nitrogen doped Graphene and ultra-thin MoSe 2composite material of nanometer sheet and preparation method thereof, high nitrogen doped Graphene/selenizing molybdenum the nanometer sheet of the present invention's synthesis possesses the premium properties such as high connductivity, high catalysis simultaneously, can be widely used on the electrode of photocatalysis and chemical catalysis, solar cell and other new forms of energy batteries, electrode material for super capacitor.
The present invention is achieved by the following technical solutions:
The present invention relates to a kind of high nitrogen doped Graphene and ultra-thin MoSe 2the preparation method of the composite material of nanometer sheet, by by being dissolved in after the molybdenum source of water and ethylene glycol, selenium source and low nitrogen-doped graphene fully mix, carrying out solvent thermal reaction, making ultra-thin MoSe under as the ethylenediamine effect of activating agent 2while on nanometer sheet homoepitaxial to Graphene, low nitrogen-doped graphene is adulterated by the degree of depth, obtain high nitrogen doped Shi Mo Xi ?ultra-thin MoSe 2nanosheet composite material.
Described low nitrogen-doped graphene be 5 ?the NH of 20mL 3h 2o (20%wt), stir and react after being heated to 90 DEG C 2 ?within 10 hours, obtain.
Described molybdenum source is four water ammonium molybdate, i.e. (NH 4) 6mo 7o 244H 2o, the content in water and ethylene glycol is 0.2 ~ 1mmol.
Described selenium source is Na 2seO 3or its hydrate, the content in water and ethylene glycol is 3 ~ 20mmol.
Described molybdenum source and selenium source mol ratio are 10 ~ 20.
The content of described ethylenediamine in water and ethylene glycol is 5 ~ 30mL.
Described water and the volume ratio of ethylene glycol are 1:1.
The temperature of described solvent thermal reaction is 180 ~ 250 DEG C, and the reaction time is 6 ~ 24 hours.
The present invention relates to high nitrogen doped Shi Mo Xi that said method prepares ?ultra-thin MoSe 2nanosheet composite material, has thickness and is 5 ~ 10nm and vertically and the ultra-thin MoSe be grown on uniformly on high nitrogen doped Graphene 2nanometer sheet, this MoSe 2length 50 ~ the 100nm of nanometer sheet, height 50 ?80nm; High nitrogen doped Graphene thickness is 1.8 ~ 2.5nm, and nitrogen content is more than 10wt%.
Technique effect
Compared with prior art, the technology of the present invention effect comprises:
1) relative to graphene oxide as initial reaction base material, there is larger suction-operated, make MoSe 2nanometer sheet together with the life of Graphene confusion, and causes MoSe 2the active edge of nanometer sheet is limited by Graphene or buries, and can not be exposed to outside, cannot play its excellent catalytic activity like this; The present invention's Graphene of low N doping, has and relatively enough adsorbs MoSe 2the active force of nanometer sheet, under the effect of surfactant, low nitrogen-doped graphene is adulterated by the degree of depth, simultaneously MoSe 2nanometer sheet is substantially vertically raw on the Graphene be as highly doped, and realizes active edge and exposes on a large scale, substantially increase the catalytic activity of composite material.
2) Graphene be as highly doped, electrical conductive activities can improve greatly, and this is because it is while being doped, and itself is also by drastic reduction, and oxy radical reduces;
3) ultra-thin MoSe 2the Graphene of nanometer sheet and high doped, the two forms a kind of novel heterojunction structure, is conducive to the transmission of electronics in electrochemical reaction process and being separated of hole, at catalysis material, solar cell, has application potential widely in ultracapacitor and lithium electricity energy storage material.
4) compared to the method for CVD and stripping, solvent heat in situ synthesis of the present invention, reaction condition controlled (temperature, time, raw material), simple to operate, laboratory apparatus is cheap, the good characteristics such as productive rate is high, favorable repeatability.
Accompanying drawing explanation
Fig. 1 is high nitrogen doped Graphene and ultra-thin MoSe in embodiment 1 2the overall SEM figure of the composite material of nanometer sheet;
Fig. 2 is the high nitrogen doped Graphene of preparation in embodiment 1 and ultra-thin MoSe 2the composite material of nanometer sheet high power SEM figure (on) and EDX distribution diagram of element (under);
Fig. 3 is the high nitrogen doped Graphene of preparation in embodiment 1 and ultra-thin MoSe 2the TEM (left side) of the composite material of nanometer sheet and HR ?TEM figure (right side);
Fig. 4 is the high nitrogen doped Graphene of preparation in embodiment 1 and ultra-thin MoSe 2the XPS figure of the composite material of nanometer sheet.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The present embodiment comprises following operating procedure:
1) preparation of the Graphene of low N doping: 500mg graphene oxide (being obtained by Hummers method) is dispersed in the 100mL aqueous solution, stirring is also ultrasonic, makes it to be uniformly dispersed; Then in dispersion liquid, add the NH of 5mL 3h 2o (20%), stirs and is heated to 90 DEG C, by chemical reaction 2 hours, obtains coarse low nitrogen Graphene; The low nitrogen Graphene of good quality is obtained finally by dialysis.
2) chemical reaction liquid is prepared: respectively by four water ammonium molybdate, the i.e. (NH of 0.2mmol 4) 6mo 7o 244H 2o and 3mmol of Na 2seO 3be dissolved in 15mL H 2in the mixed solution of O and 15mL ethylene glycol composition, stir 15 minutes;
In above-mentioned solution, add 5mL ethylenediamine (ETA) stabilizer, stir 15 minutes; The Graphene getting 5 low N doping adds above-mentioned solution, stirs and ultrasonic 30 minutes;
3) the high nitrogen doped Graphene of solvent-thermal method and ultra-thin MoSe 2the preparation of the composite material of nanometer sheet: by step 2) mixed solution for preparing adds reactor, 180 DEG C of heat treatment 6 hours, the product centrifugation obtained, and with 60 DEG C of oven dry in deionized water and absolute ethyl alcohol cyclic washing 3 times, drying box, obtain high nitrogen doped Graphene and ultra-thin MoSe 2the composite material of nanometer sheet.
Embodiment 2
The present embodiment comprises following operating procedure:
1) preparation of the Graphene of low N doping: 500mg graphene oxide (being obtained by Hummers method) is dispersed in the 100mL aqueous solution, stirring is also ultrasonic, makes it to be uniformly dispersed; Then in dispersion liquid, add the NH of 10mL 3h 2o (20%), stirs and is heated to 90 DEG C, by chemical reaction 10 hours, obtains coarse low nitrogen Graphene; The low nitrogen Graphene of good quality is obtained finally by dialysis.
2) chemical reaction liquid is prepared: respectively by four water ammonium molybdate, the i.e. (NH of 0.5mmol 4) 6mo 7o 244H 2o and 10mmol of Na 2seO 3be dissolved in 15mL H 2in the mixed solution of O and 15mL ethylene glycol composition, stir 15 minutes;
In above-mentioned solution, add 15mL ethylenediamine (ETA) stabilizer, stir 15 minutes; The Graphene getting the low N doping of 15mL adds above-mentioned solution, stirs and ultrasonic 30 minutes;
3) the high nitrogen doped Graphene of solvent-thermal method and ultra-thin MoSe 2the preparation of the composite material of nanometer sheet: by step 2) in the mixed solution for preparing add reactor, 200 DEG C of heat treatment 6 ~ 24 hours, the product centrifugation obtained, and with 60 DEG C of oven dry in deionized water and absolute ethyl alcohol cyclic washing 3 times, drying box, obtain high nitrogen doped Graphene and ultra-thin MoSe 2the composite material of nanometer sheet.
Embodiment 3
The present embodiment comprises following operating procedure:
1) preparation of the Graphene of low N doping: 500mg graphene oxide (being obtained by Hummers method) is dispersed in the 100mL aqueous solution, stirring is also ultrasonic, makes it to be uniformly dispersed; Then in dispersion liquid, add the NH of 15mL 3h 2o (20%), stirs and is heated to 90 DEG C, by chemical reaction 10 hours, obtains coarse low nitrogen Graphene; The low nitrogen Graphene of good quality is obtained finally by dialysis.
2) chemical reaction liquid is prepared: respectively by four water ammonium molybdate, the i.e. (NH of 1.5mmol 4) 6mo 7o 244H 2o and 15mmol of Na 2seO 3be dissolved in 15mL H 2in the mixed solution of O and 15mL ethylene glycol composition, stir 15 minutes;
In above-mentioned solution, add 25mL ethylenediamine (ETA) stabilizer, stir 15 minutes; The Graphene getting the low N doping of 20mL adds above-mentioned solution, stirs and ultrasonic 30 minutes;
3) the high nitrogen doped Graphene of solvent-thermal method and ultra-thin MoSe 2the preparation of the composite material of nanometer sheet: by step 2) in the mixed solution for preparing add reactor, 220 DEG C of heat treatment 12 hours, the product centrifugation obtained, and with 60 DEG C of oven dry in deionized water and absolute ethyl alcohol cyclic washing 3 times, drying box, obtain high nitrogen doped Graphene and ultra-thin MoSe 2the composite material of nanometer sheet.
Embodiment 4
The present embodiment comprises following operating procedure:
1) preparation of the Graphene of low N doping: 500mg graphene oxide (being obtained by Hummers method) is dispersed in the 100mL aqueous solution, stirring is also ultrasonic, makes it to be uniformly dispersed; Then in dispersion liquid, add the NH of 20mL 3h 2o (20%), stirs and is heated to 90 DEG C, by chemical reaction 10 hours, obtains coarse low nitrogen Graphene; The low nitrogen Graphene of good quality is obtained finally by dialysis.
2) chemical reaction liquid is prepared: respectively by four water ammonium molybdate, the i.e. (NH of 1mmol 4) 6mo 7o 244H 2o and 20mmol of Na 2seO 3be dissolved in 15mL H 2in the mixed solution of O and 15mL ethylene glycol composition, stir 15 minutes;
In above-mentioned solution, add 30mL ethylenediamine (ETA) stabilizer, stir 15 minutes; The Graphene getting the low N doping of 30mL adds above-mentioned solution, stirs and ultrasonic 30 minutes;
3) the high nitrogen doped Graphene of solvent-thermal method and ultra-thin MoSe 2the preparation of the composite material of nanometer sheet: by step 2) in the mixed solution for preparing add reactor, 250 DEG C of heat treatment 24 hours, the product centrifugation obtained, and with 60 DEG C of oven dry in deionized water and absolute ethyl alcohol cyclic washing 3 times, drying box, obtain high nitrogen doped Graphene and ultra-thin MoSe 2the composite material of nanometer sheet.
Embodiment 5
The present embodiment comprises following operating procedure:
1) preparation of the Graphene of low N doping: 500mg graphene oxide (being obtained by Hummers method) is dispersed in the 100mL aqueous solution, stirring is also ultrasonic, makes it to be uniformly dispersed; Then in dispersion liquid, add the NH of 10mL 3h 2o (20%), stirs and is heated to 90 DEG C, by chemical reaction 10 hours, obtains coarse low nitrogen Graphene; The low nitrogen Graphene of good quality is obtained finally by dialysis.
2) chemical reaction liquid is prepared: respectively by four water ammonium molybdate, the i.e. (NH of 1mmol 4) 6mo 7o 244H 2o and 20mmol of Na 2seO 3be dissolved in 15mL H 2in the mixed solution of O and 15mL ethylene glycol composition, stir 15 minutes;
In above-mentioned solution, add 25mL ethylenediamine (ETA) stabilizer, stir 15 minutes; The Graphene getting the low N doping of 30mL adds above-mentioned solution, stirs and ultrasonic 30 minutes;
3) the high nitrogen doped Graphene of solvent-thermal method and ultra-thin MoSe 2the preparation of the composite material of nanometer sheet: by step 2) in the mixed solution for preparing add reactor, 220 DEG C of heat treatment 12 hours, the product centrifugation obtained, and with 60 DEG C of oven dry in deionized water and absolute ethyl alcohol cyclic washing 3 times, drying box, obtain high nitrogen doped Graphene and ultra-thin MoSe 2the composite material of nanometer sheet.
The product that the present invention prepares according to above-described embodiment design parameter, i.e. high nitrogen doped Graphene and ultra-thin MoSe 2the composite material of nanometer sheet, its physical chemistry test experiments data are:
As shown in Figure 1, be ultra-thin MoSe 2nanometer sheet homoepitaxial is on nitrogen-doped graphene;
As shown in Figure 2, be MoSe 2nanometer sheet is perpendicular to Graphene, and its active edge exposes outwardly, and marginal dimension is below 100nm, and Mo, Se, C, N, O Elemental redistribution is even;
As shown in Figure 3, for further illustrating MoSe 2nanometer sheet is perpendicular to Graphene, and its active edge exposes outwardly, and edge thickness is below 8nm, and individual layer nanometer sheet thickness is 0.62nm;
As shown in Figure 4, be accurate Characterization Mo, Se, C, N, O constituent content, determine that N content is more than 10%.

Claims (10)

1. a high nitrogen doped Graphene and ultra-thin MoSe 2the preparation method of the composite material of nanometer sheet, is characterized in that, by by being dissolved in after the molybdenum source of water and ethylene glycol, selenium source and low nitrogen-doped graphene fully mix, carrying out solvent thermal reaction, make ultra-thin MoSe under as the ethylenediamine effect of activating agent 2while on nanometer sheet homoepitaxial to Graphene, low nitrogen-doped graphene is adulterated by the degree of depth, obtain high nitrogen doped Shi Mo Xi ?ultra-thin MoSe 2nanosheet composite material.
2. method according to claim 1, is characterized in that, described low nitrogen-doped graphene be 5 ?the NH of 20mL 3h 2o, stir and react after being heated to 90 DEG C 2 ?within 10 hours, obtain.
3. method according to claim 1, is characterized in that, described molybdenum source is four water ammonium molybdate, i.e. (NH 4) 6mo 7o 244H 2o, the content in water and ethylene glycol is 0.2 ~ 1mmol.
4. method according to claim 1, is characterized in that, described selenium source is Na 2seO 3or its hydrate, the content in water and ethylene glycol is 3 ~ 20mmol.
5. method according to claim 1, is characterized in that, described molybdenum source and selenium source mol ratio are 10 ~ 20.
6. method according to claim 1, is characterized in that, the content of described ethylenediamine in water and ethylene glycol is 5 ~ 30mL.
7. the method according to above-mentioned arbitrary claim, is characterized in that, described water and the volume ratio of ethylene glycol are 1:1.
8. method according to claim 1, is characterized in that, the temperature of described solvent thermal reaction is 180 ~ 250 DEG C, and the reaction time is 6 ~ 24 hours.
9. the ultra-thin MoSe of high nitrogen doped stone ink alkene ?that method prepares according to above-mentioned arbitrary claim 2nanosheet composite material, is characterized in that, has thickness and is 5 ~ 10nm and vertically and the ultra-thin MoSe be grown on uniformly on high nitrogen doped Graphene 2nanometer sheet, this MoSe 2length 50 ~ the 100nm of nanometer sheet, height 50 ?80nm; High nitrogen doped Graphene thickness is 1.8 ~ 2.5nm, and nitrogen content is more than 10wt%.
10. the ultra-thin MoSe of high nitrogen doped stone ink alkene ?according to above-mentioned arbitrary claim 2the application of nanosheet composite material, is characterized in that, uses it for catalysis or the electrode for the preparation of battery.
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CN105322146A (en) * 2015-09-28 2016-02-10 复旦大学 Molybdenum selenide/carbon nanofiber/graphene composite material and preparation method thereof
KR20160097026A (en) * 2015-02-06 2016-08-17 주식회사 그래핀올 Nanocomposite for secondary battery and method of producing the same
CN107275603A (en) * 2017-06-09 2017-10-20 福州大学 MoSe2The preparation of OMC compounds and its application in lithium ion battery
CN109473634A (en) * 2017-09-07 2019-03-15 南京理工大学 Solid phase heat together synthesizes two selenizing molybdenums/N doping carbon-point method
CN109794268A (en) * 2019-01-23 2019-05-24 北京科技大学 MoSe2Nanometer sheet coats KNbO3The preparation method of nano wire hetero structure catalysis material
CN114512650A (en) * 2022-02-16 2022-05-17 山东海科创新研究院有限公司 Molybdenum diselenide modified nitrogen-doped graphene composite material, preparation method thereof and nitrogen-doped graphene-based lithium-sulfur battery positive electrode material

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KR20160097026A (en) * 2015-02-06 2016-08-17 주식회사 그래핀올 Nanocomposite for secondary battery and method of producing the same
KR101655941B1 (en) 2015-02-06 2016-09-08 주식회사 그래핀올 Nanocomposite for secondary battery and method of producing the same
CN105322146A (en) * 2015-09-28 2016-02-10 复旦大学 Molybdenum selenide/carbon nanofiber/graphene composite material and preparation method thereof
CN107275603A (en) * 2017-06-09 2017-10-20 福州大学 MoSe2The preparation of OMC compounds and its application in lithium ion battery
CN109473634A (en) * 2017-09-07 2019-03-15 南京理工大学 Solid phase heat together synthesizes two selenizing molybdenums/N doping carbon-point method
CN109473634B (en) * 2017-09-07 2021-05-04 南京理工大学 Method for solid-phase co-thermal synthesis of molybdenum diselenide/nitrogen-doped carbon rod
CN109794268A (en) * 2019-01-23 2019-05-24 北京科技大学 MoSe2Nanometer sheet coats KNbO3The preparation method of nano wire hetero structure catalysis material
CN109794268B (en) * 2019-01-23 2020-09-04 北京科技大学 MoSe2Nanosheet-coated KNbO3Preparation method of nano-wire heterostructure photocatalytic material
CN114512650A (en) * 2022-02-16 2022-05-17 山东海科创新研究院有限公司 Molybdenum diselenide modified nitrogen-doped graphene composite material, preparation method thereof and nitrogen-doped graphene-based lithium-sulfur battery positive electrode material

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