CN106590815A - Preparation method of g-C3N4/MoS2 nano composite material - Google Patents
Preparation method of g-C3N4/MoS2 nano composite material Download PDFInfo
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
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- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
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- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
Abstract
The invention provides a preparation method of a g-C3N4/MoS2 nano composite material. The preparation method includes the steps of: 1) preparing g-C3N4 powder, and adding the g-C3N4 powder to deionized water and performing ultrasonic treatment to obtain a g-C3N4 dispersion liquid; 2) successively adding molybdate and hydroxylamine hydrochloride to the g-C3N4 dispersion liquid, and performing magnetic stirring for 5-10 min to obtain a mixed liquid A; 3) weighing thiourea and dissolving the thiourea in deionized water to prepare a thiourea solution, dropwise adding the thiourea solution to the mixed liquid A by a dropper, and continuously stirring the mixture for 5-10 min to obtain a mixed liquid B; 4) moving the mixed liquid B to a hydrothermal reaction kettle with polytetrafluoroethylene as a liner to perform a reaction, and after the reaction is finished, naturally cooling the reaction product to room temperature, and centrifuging and collecting the reaction product, washing the product in deionized water and anhydrous ethanol, and drying the product to prepare the g-C3N4/MoS2 nano composite material. The method is simple and controllable and has mild reaction conditions, high yield and good repeatability. The g-C3N4/MoS2 nano composite material has uniform particle size and good dispersibility.
Description
Technical field
The invention belongs to field of nanocomposite materials, specifically discloses a kind of g-C3N4/MoS2The preparation of nano composite material
Method.
Background technology
In recent years, transition metal chalcogenide MX2(M=Mo, W, Nb etc.；X=S, Se, Te), due to its unique physics
The structure of chemical property and novelty, gets more and more people's extensive concerning and furthers investigate, and these materials are widely used as lithium-ion electric
Pond electrode, lube oil additive, new catalyst and thermoelectric material etc., wherein, MoS2As in transition metal chalcogenide
Important a member, due to its special hexagonal layered structure, and many peculiar properties are made it have, in MoS2Crystal
In structure, by strong chemical bonds in S-Mo-S layers, and combined by weak Van der Waals force between layers, layer and layer
It is easy to peel off, with good anisotropy and relatively low coefficient of friction.MoS with nanostructured2In many performances
Have been further upgraded, highlightedly show the following aspects：Greatly, adsorption capacity is higher, reactivity for specific surface area
Height, the performance of catalytic performance especially catalytic hydrogenation desulfurization is higher, can be used to prepare special catalysis material and gas storing material；Nanometer
MoS2The close 1.78eV of band difference of thin layer, matches with the energy of light, has application prospect on photocell material；With MoS2
Particle diameter diminish, it is all significantly improved in the tack and level of coverage of friction material surface, and wear-resistant, antifriction performance is also obtained into
Improve again.
g-C3N4It is a kind of polymer semiconductor similar to graphene-structured, C, N atom is with sp2Hydridization formed height from
The pi-conjugated system in domain.g-C3N4Not only there is wide material sources, the relatively low advantage of price of polymeric material, and its excellent light is urged
Change performance also can compare favourably with traditional inorganic semiconductor catalysis material.g-C3N4Because of its unique band structure and excellent change
Stability is learned, and has certain absorption to visible ray, with preferable photocatalysis performance, therefore be widely used as photochemical catalyst, such as
Photocatalysis degradation organic contaminant, photocatalysis liberation of hydrogen and photocatalysis organic synthesis etc..Additionally, researcher employs pattern tune
The strategies such as control, element doping, semiconductors coupling, effectively increase its photocatalytic activity.Recent studies have shown that, g-C3N4Can increase
Original performance of strong composite, therefore g-C3N4Based nano composite material lithium electricity, fuel sensitized cells, ultracapacitor and
The fields such as lubrication have potential application prospect.g-C3N4Although can not be compared with Graphene in intensity, it can be gentle
Under conditions of carried out by a series of predecessor (melamine etc.) of carbon containings richness nitrogen it is a large amount of synthetically prepared, the stability of its height,
Unique electronic structure and class graphene film Rotating fields make its lubrication, catalyst carrier, sensor, organic reaction catalyst,
The aspects such as photochemical catalyst, gas storage have very huge potential using value, and are seen as most being hopeful to supplement carbon materials
Expect the material in many aspect potential applications, thus cause Chinese scholars and researcher to this with unlimited potentiality
The tireless exploration of new material.
Based on g-C3N4、MoS2Good characteristic, g-C3N4/MoS2Nano composite material can show relative its homogenous material
More comprehensive, excellent performance.For nano composite material, at present mostly research concentrates on graphene-based nano combined material
The multiple material of material, such as Graphene/molybdenum disulfide nano, and in g-C3N4The research in based nano composite material field is less, and focuses mostly on
Research is with g-C3N4For the composite of main component.Therefore, the invention discloses one kind is with MoS2For the g-C of main body3N4/MoS2
The preparation method of nano composite material, and there is good development prospect in fields such as tribology, catalysis, lithium electricity.
The content of the invention
It is an object of the invention to provide a kind of g-C3N4/MoS2The preparation method of nano composite material, to improve curing
The performances such as the electricity of molybdenum, calorifics, catalysis and tribology and extend its application.
The present invention is achieved through the following technical solutions：
A kind of g-C3N4/MoS2The preparation method of nano composite material, comprises the steps：
The preparation of step 1, g-C3N4 dispersion liquids：
Prepare g-C3N4Powder, then by g-C3N4Powder is added in deionized water, ultrasonically treated, and g-C is obtained3N4Dispersion
Liquid；
Step 2, g-C3N4/MoS2The preparation of nano composite material：
First, successively molybdate, hydroxylamine hydrochloride be added to into step 1 gained g-C3N4In dispersion liquid, magnetic agitation 5～
10min, obtains mixed liquor A；
Then, weigh thiocarbamide to be dissolved in deionized water, thiourea solution is obtained, be dropwise added drop-wise in mixed liquor A with dropper, and
5～10min is stirred continuously, mixed liquid B is obtained；
Finally, mixed liquid B is moved into into polytetrafluoroethylene (PTFE) to react in the hydrothermal reaction kettle of liner, it is natural after reaction terminates
Room temperature is cooled to, product is collected by centrifugation, deionized water and absolute ethyl alcohol are washed to product, be dried, obtain g-C3N4/
MoS2Nano composite material.
In step 1, the g-C3N4The preparation method of powder is：With urea as raw material, 10g urea is placed in into the band of 25mL
In lid corundum crucible, in being transferred to chamber type electric resistance furnace, with 10～20 DEG C/min temperature programmings to 550～600 DEG C, 2h is incubated, from
Room temperature is so cooled to, faint yellow g-C is obtained3N4Powder.
In step 1, the sonication treatment time is 30～60min, the g-C3N4The concentration of dispersion liquid is 0.5～4mg/
mL。
In step 2, the molybdate is sodium molybdate or ammonium molybdate；When using ammonium molybdate, the ammonium molybdate is in mixed liquor A
In concentration be 5.515mg/mL, ammonium molybdate：Thiocarbamide：The mol ratio of hydroxylamine hydrochloride is 1：14：15.4；When using sodium molybdate,
Concentration of the sodium molybdate in mixed liquor A be 7.555mg/mL, sodium molybdate：Thiocarbamide：The mol ratio 1 of hydroxylamine hydrochloride：2：2.2.
In step 2, the concentration of the thiourea solution is 0.2499mmol/mL, and drop rate is 1 drop/sec.
In step 2, the reaction kettle for reaction condition is 180～220 DEG C, and the reaction time is 24h.
In step 2, the drying condition is dried 12h for 60 DEG C.
Prepared g-C3N4/MoS2In nano composite material, g-C3N4Mass fraction be 9%～50%.
Beneficial effects of the present invention are：
Method provided by the present invention, simple production process is easily-controllable, and reaction condition is gentle, and yield is high and favorable reproducibility, system
The g-C of standby gained3N4/MoS2Nano-complex grain size is uniform, good dispersion, can be applicable to lube oil additive, hydrogen storage,
The fields such as photocatalysis, have a good application prospect.Especially, the g-C of graphite-phase3N4It is with lamellar structure lightweight two dimension material
Material, has good lubricity and dispersiveness concurrently, meanwhile, MoS2Ultrathin nanometer piece is typical lubriation material, both " collaboration works
With " more preferably antifriction antiwear effect can be played.
Description of the drawings
Fig. 1 is the g-C of the synthesis of example 13N4SEM figure.
Fig. 2 is MoS in example 22And the g-C of synthesis3N4With g-C3N4/MoS2The XRD of nano composite material.
Fig. 3 is the g-C of the synthesis of example 33N4/MoS2Nano composite material SEM is schemed, wherein figure (b) is put for the local of figure (a)
Big figure.
Fig. 4 is the g-C of the synthesis of example 43N4/MoS2Nano composite material EDS is schemed.
Fig. 5 is the g-C of the synthesis of example 43N4/MoS2Nano composite material XPS is schemed.
Fig. 6 is the g-C of the synthesis of example 53N4/MoS2Nano composite material TEM is schemed.
Fig. 7 is the g-C synthesized in example 23N4/MoS2The friction coefficient curve figure of nano composite material.
Specific embodiment
Present disclosure is further illustrated below in conjunction with example, as known by the technical knowledge, the present invention can also pass through other
The scheme without departing from the technology of the present invention feature it is describing therefore all within the scope of the present invention or in the equivalent scope of the invention
Change is included in the invention.
Ammonium molybdate chemical formula used in the present invention is (NH4)6Mo7O24·4H2O, molecular weight is 1235.86；Molybdic acid sodium
Formula is Na2MoO4·2H2O, molecular weight is 241.95；Hydroxylamine hydrochloride chemical formula is HONH3Cl, molecular weight is 69.49；Thiocarbamide
Chemical formula is CH4N2S, molecular weight is 76.12.
Embodiment 1：
(1)g-C3N4Preparation：
With urea as raw material, 10g urea is placed in the corundum crucible with cover of 25mL, in being transferred to chamber type electric resistance furnace, is risen
To 550 DEG C, programming rate is 10 DEG C/min to temperature, is incubated 2h, naturally cools to room temperature, obtains faint yellow g-C3N4Powder.
(2)g-C3N4/MoS2The preparation of nano composite material：
Weigh obtained g-C in step (1)3N4Powder 0.02g is added in 40mL deionized waters, ultrasonically treated 30min,
Prepared concentration is the dispersion liquid of 0.5mg/mL；Then according to ammonium molybdate：Hydroxylamine hydrochloride=1：15.4 mol ratio weighs successively molybdenum
Sour ammonium 0.2206g, hydroxylamine hydrochloride 0.1910g are added to g-C3N4In dispersion liquid, magnetic agitation 5min；Then, according to ammonium molybdate：
Thiocarbamide=1：14 mol ratio weighs thiocarbamide 0.1902g, in being dissolved in 10mL deionized waters, the thiocarbamide of 0.2499mmol/mL is obtained
Solution, is dropwise added drop-wise in above-mentioned dispersion liquid and is stirred continuously 5min with dropper with 1 drop/sec of speed, finally moves mixed liquor
In entering the hydrothermal reaction kettle that polytetrafluoroethylene (PTFE) is liner, hydro-thermal 24h under conditions of 180 DEG C naturally cooled to and be centrifuged after room temperature
Product is collected, deionized water and absolute ethyl alcohol wash to product, be finally dried 12h at 60 DEG C and obtain g-C3N4/MoS2
Nano composite material.
The SEM figures of Fig. 1 are it can be seen that the g-C for preparing3N4Lamellar structure with class Graphene.
Embodiment 2：
(1)g-C3N4Preparation：
With urea as raw material, 10g urea is placed in the corundum crucible with cover of 25mL, in being transferred to chamber type electric resistance furnace, is risen
To 570 DEG C, programming rate is 15 DEG C/min to temperature, is incubated 2h, naturally cools to room temperature, obtains faint yellow g-C3N4Powder.
(2)g-C3N4/MoS2The preparation of nano composite material：
Weigh obtained g-C in step (1)3N4Powder 0.08g is added in 40mL deionized waters, ultrasonically treated 40min,
Prepared concentration is the dispersion liquid of 2mg/mL, then according to ammonium molybdate：Hydroxylamine hydrochloride=1：15.4 mol ratio weighs successively molybdic acid
Ammonium 0.2206g, hydroxylamine hydrochloride 0.1910g are added to g-C3N4In dispersion liquid, magnetic agitation 10min；Then, according to ammonium molybdate：Sulphur
Urea=1：14 mol ratio weighs thiocarbamide 0.1902g and is dissolved in 10mL deionized waters, and 0.2499mmol/ml thiourea solutions are obtained,
10min is dropwise added drop-wise in above-mentioned dispersion liquid and is stirred continuously with 1 drop/sec of speed with dropper, is finally moved into mixed liquor poly-
During tetrafluoroethene is for the hydrothermal reaction kettle of liner, hydro-thermal 24h under conditions of 200 DEG C naturally cooled to and be collected by centrifugation after room temperature
Product, deionized water and absolute ethyl alcohol are washed to product, are finally dried 12h at 60 DEG C and are obtained g-C3N4/MoS2Nanometer
Composite.
The XRD spectrum of Fig. 2 can be seen that the g-C of synthesis3N4With higher purity, simultaneously synthesizing nano composite material
There is g-C simultaneously3N4、MoS2Exist, tentatively illustrate g-C3N4/MoS2The successful preparation of nano composite material.
Embodiment 3：
(1)g-C3N4Preparation：
With urea as raw material, 10g urea is placed in the corundum crucible with cover of 25mL, in being transferred to chamber type electric resistance furnace, is risen
To 570 DEG C, programming rate is 15 DEG C/min to temperature, is incubated 2h, naturally cools to room temperature, obtains faint yellow g-C3N4Powder.
(2)g-C3N4/MoS2The preparation of nano composite material：
Weigh obtained g-C in step (1)3N4Powder 0.08g is added in 40mL deionized waters, ultrasonically treated 50min,
Prepared concentration is the dispersion liquid of 2mg/mL, then according to sodium molybdate：Hydroxylamine hydrochloride=1：2.2 mol ratio weighs successively sodium molybdate
0.3022g, hydroxylamine hydrochloride 0.1910g are added to g-C3N4In dispersion liquid, magnetic agitation 5min；Then, according to sodium molybdate：Thiocarbamide
=1：2 mol ratio weighs thiocarbamide 0.1902g, in being dissolved in 10mL deionized waters, the thiourea solution of 0.2499mmol/mL is obtained,
5min is dropwise added drop-wise in above-mentioned dispersion liquid and is stirred continuously with 1 drop/sec of speed with dropper, finally mixed liquor poly- four is moved into into
During PVF is for the hydrothermal reaction kettle of liner, hydro-thermal 24h under conditions of 200 DEG C is naturally cooled to and be collected by centrifugation after room temperature product
Thing, deionized water and absolute ethyl alcohol are washed to product, are finally dried 12h at 60 DEG C and are obtained g-C3N4/MoS2Nanometer is multiple
Condensation material.
The SEM figures of Fig. 3 are it can be seen that the g-C for preparing3N4/MoS2With ideal binary heterojunction structure, further
Illustrate g-C3N4With MoS2Define more perfect composite construction.
Embodiment 4：
(1)g-C3N4Preparation：
With urea as raw material, 10g urea is placed in the corundum crucible with cover of 25mL, in being transferred to chamber type electric resistance furnace, is risen
To 600 DEG C, programming rate is 20 DEG C/min to temperature, is incubated 2h, naturally cools to room temperature, obtains faint yellow g-C3N4Powder.
(2)g-C3N4/MoS2The preparation of nano composite material：
Weigh obtained g-C in step (1)3N4Powder 0.16g is added in 40mL deionized waters, ultrasonically treated 60min,
Prepared concentration is the dispersion liquid of 4mg/mL, then according to ammonium molybdate：Hydroxylamine hydrochloride=1：15.4 mol ratio weighs successively molybdic acid
Ammonium 0.2206g, hydroxylamine hydrochloride 0.1910g are added to g-C3N4In dispersion liquid, magnetic agitation 10min；Then, according to ammonium molybdate：Sulphur
Urea=1：14 mol ratio weighs thiocarbamide 0.1902g and is dissolved in 10mL deionized waters, and 0.2499mmol/ml thiourea solutions are obtained,
8min is dropwise added drop-wise in above-mentioned dispersion liquid and is stirred continuously with 1 drop/sec of speed with dropper, finally mixed liquor poly- four is moved into into
During PVF is for the hydrothermal reaction kettle of liner, hydro-thermal 24h under conditions of 220 DEG C is naturally cooled to and be collected by centrifugation after room temperature product
Thing, deionized water and absolute ethyl alcohol are washed to product, are finally dried 12h at 60 DEG C and are obtained g-C3N4/MoS2Nanometer is multiple
Condensation material.
The EDS collection of illustrative plates of Fig. 4 can be seen that the g-C of preparation3N4/MoS2It is any miscellaneous without other with C, N, Mo, S element
Prime element, the full spectrum of XPS detections of Fig. 5 also finds out that the material of synthesis is made up of Mo, S, N, C element, and Mo, S molar ratio and C, N rub
That ratio is all close to MoS2、g-C3N4Stoichiometric proportion, illustrate synthesize heterojunction structure be strictly by MoS2、g-C3N4Group
Into.
Embodiment 5：
(1)g-C3N4Preparation：
With urea as raw material, 10g urea is placed in the corundum crucible with cover of 25mL, in being transferred to chamber type electric resistance furnace, is risen
To 550 DEG C, programming rate is 15 DEG C/min to temperature, is incubated 2h, naturally cools to room temperature, obtains faint yellow g-C3N4Powder.
(2)g-C3N4/MoS2The preparation of nano composite material：
Weigh obtained g-C3N4 powder 0.12g in step (1) to be added in 40mL deionized waters, ultrasonically treated 50min,
Prepared concentration is the dispersion liquid of 3mg/mL, then according to sodium molybdate：Hydroxylamine hydrochloride=1：2.2 mol ratio weighs successively sodium molybdate
0.3022g, hydroxylamine hydrochloride 0.1910g are added to g-C3N4In dispersion liquid, magnetic agitation 5min；Then, according to sodium molybdate：Thiocarbamide
=1：2 mol ratio weighs thiocarbamide 0.1902g, in being dissolved in 8mL deionized waters, the thiourea solution of 0.2499mmol/mL is obtained, and uses
Dropper is dropwise added drop-wise in above-mentioned dispersion liquid and is stirred continuously 5min with 1 drop/sec of speed, finally mixed liquor is moved into into polytetrafluoro
During ethene is for the hydrothermal reaction kettle of liner, hydro-thermal 24h under conditions of 200 DEG C is naturally cooled to and be collected by centrifugation after room temperature product,
Deionized water and absolute ethyl alcohol are washed to product, are finally dried 12h at 60 DEG C and are obtained g-C3N4/MoS2It is nano combined
Material.
The TEM figures of Fig. 6 further can clearly find out the g-C of preparation3N4/MoS2Nano composite material has ideal
Binary hetero-junctions pattern, g-C3N4Nanometer sheet surface appendix has MoS2Nano flake, and g-C3N4Space steric effect promote
Make MoS2There is not flower ball-shaped structure.
Embodiment 6：
By g-C prepared in example 23N4/MoS2Nano composite material is added in lubricating base oils carries out friction in fact
Test, and with base oil, g-C3N4, molybdenum bisuphide compares.Frictional experiment is on CETR UMT-2 multifunction friction wear testing machines
Carry out.Using ball-disc type contact, a diameter of 4mm of stainless steel ball.Experiment load is 30N, and speed of experiment is 100r/min (revolutions
Radius r=3mm).By prepared g-C3N4/MoS2、g-C3N4And MoS2Base oil is added according to 1% mass percent
In HVI750, and the base oil HVI750 of the lubricant ultrasonic disperse 2h in ultrasonic washing instrument is not added with.Frictional experiment is tested
As a result as shown in fig. 7, as seen from the figure, g-C3N4、MoS2With the g-C prepared by the present invention3N4/MoS2Nano composite material exists
Obvious antifriction effect, but the g-C prepared by the present invention are respectively provided with during as lube oil additive3N4/MoS2Nano composite material
Than simple g-C3N4、MoS2With more preferable tribological property.
Claims (8)
1. a kind of g-C3N4/MoS2The preparation method of nano composite material, it is characterised in that comprise the steps：
The preparation of step 1, g-C3N4 dispersion liquids：
Prepare g-C3N4Powder, then by g-C3N4Powder is added in deionized water, ultrasonically treated, and g-C is obtained3N4Dispersion liquid；
Step 2, g-C3N4/MoS2The preparation of nano composite material：
First, successively molybdate, hydroxylamine hydrochloride be added to into step 1 gained g-C3N4In dispersion liquid, 5～10min of magnetic agitation is obtained
Mixed liquor A；
Then, weigh thiocarbamide to be dissolved in deionized water, thiourea solution is obtained, be dropwise added drop-wise in mixed liquor A with dropper, and constantly
5～10min of stirring, obtains mixed liquid B；
Finally, mixed liquid B is moved into into polytetrafluoroethylene (PTFE) to react in the hydrothermal reaction kettle of liner, after reaction terminates, natural cooling
To room temperature, product is collected by centrifugation, deionized water and absolute ethyl alcohol are washed to product, is dried, obtain g-C3N4/MoS2Receive
Nano composite material.
2. a kind of g-C according to claim 13N4/MoS2The preparation method of nano composite material, it is characterised in that step
In 1, the g-C3N4The preparation method of powder is：With urea as raw material, 10g urea is placed in the corundum crucible with cover of 25mL,
In being transferred to chamber type electric resistance furnace, with 10～20 DEG C/min temperature programmings to 550～600 DEG C, 2h is incubated, naturally cools to room temperature,
Obtain faint yellow g-C3N4Powder.
3. a kind of g-C according to claim 13N4/MoS2The preparation method of nano composite material, it is characterised in that step
In 1, the sonication treatment time is 30～60min, the g-C3N4The concentration of dispersion liquid is 0.5～4mg/mL.
4. a kind of g-C according to claim 13N4/MoS2The preparation method of nano composite material, it is characterised in that step
In 2, the molybdate is sodium molybdate or ammonium molybdate；When using ammonium molybdate, concentration of the ammonium molybdate in mixed liquor A is
5.515mg/mL, ammonium molybdate：Thiocarbamide：The mol ratio of hydroxylamine hydrochloride is 1：14：15.4；When using sodium molybdate, sodium molybdate is mixed
Close liquid A in concentration be 7.555mg/mL, sodium molybdate：Thiocarbamide：The mol ratio 1 of hydroxylamine hydrochloride：2：2.2.
5. a kind of g-C according to claim 13N4/MoS2The preparation method of nano composite material, it is characterised in that step
In 2, the concentration of the thiourea solution is 0.2499mmol/mL, and drop rate is 1 drop/sec.
6. a kind of g-C according to claim 13N4/MoS2The preparation method of nano composite material, it is characterised in that step
In 2, the reaction kettle for reaction condition is 180～220 DEG C, and the reaction time is 24h.
7. a kind of g-C according to claim 13N4/MoS2The preparation method of nano composite material, it is characterised in that step
In 2, the drying condition is dried 12h for 60 DEG C.
8. a kind of g-C according to claim 13N4/MoS2The preparation method of nano composite material, it is characterised in that made
Standby g-C3N4/MoS2In nano composite material, g-C3N4Mass fraction be 9%～50%.
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