CN106430288A - Preparation method of g-C3N4/ZnS nano composite material - Google Patents
Preparation method of g-C3N4/ZnS nano composite material Download PDFInfo
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Abstract
The invention provides a preparation method of a g-C3N4/ZnS nano composite material. The preparation method includes: 1, preparing a g-C3N4 dispersion: preparing g-C3N4 powder, adding the g-C3N4 powder into deionized water, and performing ultrasonic treatment to obtain the g-C3N4 dispersion; 2, preparing the g-C3N4/ZnS nano composite material: sequentially adding zinc acetate, sodium sulfide and urea into the g-C3N4 dispersion obtained in the step 1, magnetically stirring for 5-10min to obtain mixed liquid, transferring the mixed liquid into a hydrothermal reaction kettle with polytef as lining for reaction, naturally cooling to room temperature after reaction is finished, centrifuging and collecting a product, using deionized water and anhydrous alcohol to wash the product, and drying to obtain the g-C3N4/ZnS nano composite material. The preparation method is simple and easy-to-control in production process, mild in reaction condition and high in yield and repeatability, and the g-C3N4/ZnS nano composite material prepared by the method is uniform in particle size and high in dispersity and can be applied in the field of lubricating oil additives, photoelectric materials, hydrogen storage and photocatalysis.
Description
Technical field
The invention belongs to field of nanocomposite materials, specifically discloses a kind of g-C3N4The preparation of/ZnS 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
Chemical property and novel structure, get more and more people's extensive concerning and further investigate, and these materials are widely used as lithium-ion electric
Pond electrode, lube oil additive, new catalyst and thermoelectric material etc., wherein, ZnS is used as the one of transition metal chalcogenide
Member, is II-VI race wide bandgap semiconductor compound-material, and its Emission in Cubic energy gap is that 3.7eV, hexagonal phase energy gap is
3.8eV.Used as a kind of semi-conducting material, ZnS is sent out in flat faced display, electroluminescent, device for non-linear optical, cathode ray
Light, light emitting diode, field-effect transistor, solaode, dielectric filter, infrared window material, dyestuff, photocatalysis, sensor
And laser, the aspect such as solid lubrication suffers from being widely applied.When the particle diameter of ZnS particle is less than the Bohr radius of its exciton,
It can present obvious quantum size effect, and its photoelectricity, frictional behaviour also can be with the changes of size and pattern
Change.Therefore, the preparation of ZnS and performance study cause the broad interest of Chinese scholars.So far, lot of domestic and foreign section
Grind group and passed through different synthetic methods and successfully synthesize ZnS nanometer rods, nano wire, nanometer sheet, nano belt, nanotube, receive
The low-dimension nano materials such as rice grain.
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 to 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, be therefore widely used as photocatalyst, such as
Photocatalysis degradation organic contaminant, photocatalysis liberation of hydrogen and photocatalysis organic synthesiss etc..Additionally, research worker 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, which can be gentle
Under conditions of by a series of carbon containings richness nitrogen predecessor (tripolycyanamide etc.) carry out synthetically prepared in a large number, 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 photocatalyst, gas storage have very huge potential using value, and are seen as most being hopeful to supplement carbon materials
Expecting the material in a lot of aspect potential applications, Chinese scholars and research worker is thus caused to this with unlimited potentiality
The tireless exploration of new material.
Based on g-C3N4, ZnS good characteristic, g-C3N4/ ZnS nano composite material can show its homogenous material relative
More comprehensive, excellent performance.For nano composite material, research concentrates on graphene-based nano combined material mostly at present
The multiple material of material, such as Graphene/molybdenum disulfide nano, and in g-C3N4The research in based nano composite material field is less.Therefore, originally
A kind of g-C of disclosure of the invention3N4The preparation method of/ZnS bielement nano composite, and in fields such as tribology, catalysis, lithium electricity
With good development prospect.
Content of the invention
It is an object of the invention to provide a kind of g-C3N4The preparation method of/ZnS ternary nano composite material, to improve sulfur
Change the performances such as electricity, calorifics, catalysis and the tribology of zinc and extend its application.
The present invention is achieved through the following technical solutions：
A kind of g-C3N4The preparation method of/ZnS nano composite material, comprises the steps：
Step 1, g-C3N4The preparation of dispersion liquid：
First preparation g-C3N4Powder, then by g-C3N4Powder is added in deionized water, supersound process, prepared g-C3N4Point
Dispersion liquid；
Step 2, g-C3N4The preparation of/ZnS nano composite material：
First, successively zinc acetate, sodium sulfide, carbamide are added to step 1 gained g-C3N4In dispersion liquid, magnetic agitation 5～
10min, obtains mixed liquor；Subsequently, mixed liquor is moved into and reacts in hydrothermal reaction kettle of the politef for liner, reaction terminates
Afterwards, room temperature is naturally cooled to, product is collected by centrifugation, deionized water and dehydrated alcohol are washed to product, dry；Finally,
Obtain g-C3N4/ ZnS nano composite material.
In step 1, the g-C3N4The preparation method of powder is：With carbamide as raw material, 10g carbamide is placed in the band of 25mL
In lid corundum crucible, it is transferred in chamber type electric resistance furnace, with 10～20 DEG C/min temperature programming to 550～600 DEG C, 2h is incubated, from
So room temperature is cooled to, obtains faint yellow g-C3N4Powder.
In step 2, the zinc acetate：The mol ratio of sodium sulfide is 1：1；Zinc unit in the carbamide of the interpolation and zinc acetate
The ratio of the element sulphur gross mass in element, sodium sulfide is 1：2～4, concentration of the carbamide in mixed liquor is 0.5～5mg/mL.
In step 2, it is 24h in 160～200 DEG C, response time that the reaction kettle for reaction condition is.
In step 2, the drying condition dries 12h for 60 DEG C.
Prepared g-C3N4In/ZnS nano composite material, g-C3N4Mass fraction be 50%～80%.
Beneficial effects of the present invention are：
Method provided by the present invention, simple production process is easily-controllable, and reaction condition is gentle, the high and favorable reproducibility of yield, system
The g-C of standby gained3N4/ ZnS nano-complex grain size is uniform, and good dispersion can be applicable to lube oil additive, photoelectricity material
The fields such as material, hydrogen storage, photocatalysis, have a good application prospect.
Description of the drawings
Fig. 1 is the g-C of the synthesis of example 13N4SEM figure.
Fig. 2 is the g-C for synthesizing in example 23N4With g-C3N4The XRD figure of/ZnS nano composite material.
Fig. 3 is the g-C of the synthesis of example 33N4The SEM figure of/ZnS nano composite material difference up-sizing.
Fig. 4 is the g-C of the synthesis of example 33N4/ ZnS nano composite material EDS is schemed.
Fig. 5 is the g-C of the synthesis of example 43N4/ ZnS nano composite material TEM is schemed.
Fig. 6 is the g-C for synthesizing in example 23N4The coefficient of friction figure of/ZnS nano composite material.
Specific embodiment
Carbamide chemical formula used in the present invention is CO (NH2)2, molecular weight is 60.06；Zinc source is zinc acetate, and chemical formula is
C4H6O4Zn·2H2O, molecular weight is 219.51；Sulphur source is sodium sulfide, and chemical formula is Na2S·9H2O, molecular weight is 240.18.
Embodiment 1：
(1)g-C3N4Preparation：
With carbamide as raw material, 10g carbamide is placed in the corundum crucible with cover of 25mL, is transferred in chamber type electric resistance furnace, rise
Temperature is to 550 DEG C, and programming rate is 10 DEG C/min, is incubated 2h, naturally cools to room temperature, obtain faint yellow g-C3N4Powder.
(2)g-C3N4The preparation of/ZnS nano composite material：
Weigh obtained g-C in step (1)3N4Powder 0.16g (50%) is added in 40mL deionized water, supersound process
30min, prepared concentration is the dispersion liquid of 4mg/mL；Then, according to zinc acetate：Sodium sulfide=1：1 mol ratio weighs zinc acetate
0.3604g, sodium sulfide 0.3944g, according to the ratio of the zinc element in carbamide and zinc acetate, element sulphur gross mass in sodium sulfide be
1：2 weigh carbamide 0.08g, are added to g-C3N4In dispersion liquid, 5～10min of magnetic agitation, obtain mixed liquor；Finally, by mixed liquor
Politef is moved into in the hydrothermal reaction kettle of liner, hydro-thermal 24h under conditions of 160 DEG C, naturally cool to after room temperature from
The heart collects product, and deionized water and dehydrated alcohol are washed to product, are finally dry 12h at 60 DEG C and are obtained g-C3N4/
ZnS nano composite material.
The SEM figure of Fig. 1 is it can be seen that the g-C of preparation3N4Lamellar structure with class Graphene, thickness is within 100nm.
Embodiment 2：
(1)g-C3N4Preparation：
With carbamide as raw material, 10g carbamide is placed in the corundum crucible with cover of 25mL, is transferred in chamber type electric resistance furnace, rise
Temperature is to 570 DEG C, and programming rate is 15 DEG C/min, is incubated 2h, naturally cools to room temperature, obtain faint yellow g-C3N4Powder.
(2)g-C3N4The preparation of/ZnS nano composite material：
Weigh obtained g-C in step (1)3N4Powder 0.24g (60%) is added in 40mL deionized water, supersound process
30min, prepared concentration is the dispersion liquid of 6mg/mL；Then, according to zinc acetate：Sodium sulfide=1：1 mol ratio weighs zinc acetate
0.3604g, sodium sulfide 0.3944g, according to the ratio of the zinc element in carbamide and zinc acetate, element sulphur gross mass in sodium sulfide be
1：4 weigh carbamide 0.04g, are added to g-C3N4In dispersion liquid, 5～10min of magnetic agitation, obtain mixed liquor；Finally, by mixed liquor
Politef is moved into in the hydrothermal reaction kettle of liner, hydro-thermal 24h under conditions of 180 DEG C, naturally cool to after room temperature from
The heart collects product, and deionized water and dehydrated alcohol are washed to product, are finally dry 12h at 60 DEG C and are obtained g-C3N4/
ZnS nano composite material.
The XRD spectrum of Fig. 2 can be seen that the g-C of synthesis3N4There is higher purity, simultaneously synthesizing nano composite material
Collection of illustrative plates in, ZnS has higher degree of crystallinity, and the g-C that still withs a hook at the end3N4Peak, illustrate that two kinds of materials are present, preliminary explanation
g-C3N4The successful synthesis of/ZnS.
Embodiment 3：
(1)g-C3N4Preparation：
With carbamide as raw material, 10g carbamide is placed in the corundum crucible with cover of 25mL, is transferred in chamber type electric resistance furnace, rise
Temperature is to 580 DEG C, and programming rate is 15 DEG C/min, is incubated 2h, naturally cools to room temperature, obtain faint yellow g-C3N4Powder.
(2)g-C3N4The preparation of/ZnS nano composite material：
Weigh obtained g-C in step (1)3N4Powder 0.32g (70%) is added in 40mL deionized water, supersound process
30min, prepared concentration is the dispersion liquid of 8mg/mL；Then, according to zinc acetate：Sodium sulfide=1：1 mol ratio weighs zinc acetate
0.3090g, sodium sulfide 0.3380g, according to the ratio of the zinc element in carbamide and zinc acetate, element sulphur gross mass in sodium sulfide be
1：2 weigh carbamide 0.069g, are added to g-C3N4In dispersion liquid, 5～10min of magnetic agitation, obtain mixed liquor；Finally, by mixed liquor
Politef is moved into in the hydrothermal reaction kettle of liner, hydro-thermal 24h under conditions of 180 DEG C, naturally cool to after room temperature from
The heart collects product, and deionized water and dehydrated alcohol are washed to product, are finally dry 12h at 60 DEG C and are obtained g-C3N4/
ZnS nano composite material.
The SEM figure of Fig. 3 is it can be seen that the g-C of preparation3N4/ ZnS has ideal 2D/3D heterojunction structure, block shape
G-C3N4Surface is thickly dotted to be loaded with a large amount of ZnS nano-particle, and granule is uniform, in spherical.
The EDS collection of illustrative plates of Fig. 4 can be seen that the g-C of preparation3N4/ ZnS has C, N, Zn, S element, does not have other any miscellaneous
Prime element.
Embodiment 4：
(1)g-C3N4Preparation：
With carbamide as raw material, 10g carbamide is placed in the corundum crucible with cover of 25mL, is transferred in chamber type electric resistance furnace, rise
Temperature is to 600 DEG C, and programming rate is 20 DEG C/min, is incubated 2h, naturally cools to room temperature, obtain faint yellow g-C3N4Powder.
(2)g-C3N4The preparation of/ZnS nano composite material：
Weigh obtained g-C in step (1)3N4Powder 0.32g (80%) is added in 40mL deionized water, supersound process
30min, prepared concentration is the dispersion liquid of 8mg/mL；Then, according to zinc acetate：Sodium sulfide=1：1 mol ratio weighs zinc acetate
0.1802g, sodium sulfide 0.1972g, according to the ratio of the zinc element in carbamide and zinc acetate, element sulphur gross mass in sodium sulfide be
1：4 weigh carbamide 0.02g, are added to g-C3N4In dispersion liquid, 5～10min of magnetic agitation, obtain mixed liquor；Finally, by mixed liquor
Politef is moved into in the hydrothermal reaction kettle of liner, hydro-thermal 24h under conditions of 200 DEG C, naturally cool to after room temperature from
The heart collects product, and deionized water and dehydrated alcohol are washed to product, are finally dry 12h at 60 DEG C and are obtained g-C3N4/
ZnS nano composite material.
The TEM figure of Fig. 5 can clearly find out the g-C of preparation further3N4/ ZnS nano composite material has ideal
Hetero-junctions pattern, g-C3N4Nanometer sheet surface appendix has ZnS nanoparticle, and granule is in spherical, and particle diameter is in 20-30nm.
Embodiment 5：
By prepared g-C in example 23N4/ ZnS nanometer self-lubricating composite is added in lubricating base oils and is rubbed
Wipe experiment, and with pure base oil, g-C3N4, zinc sulfide compares.Frictional experiment is tested in CETR UMT-2 multifunction friction wear
Carry out on machine.Using ball-disc type contact, a diameter of 4mm of stainless steel ball.Experiment load is 10N, and speed of experiment is 100r/min
(radius of gyration r=3mm).By prepared g-C3N4/ZnS、g-C3N4Basis is added with ZnS according to certain mass percent
In oily HVI750, and the base oil HVI750 of lubricant ultrasonic disperse 2h in ultrasonic washing instrument is not added with.Frictional experiment is surveyed
Test result as shown in fig. 6, as seen from the figure, g-C3N4With ZnS and g-C prepared by the present invention3N4/ ZnS nano composite material
It is respectively provided with obvious antifriction effect when as lube oil additive, but the g-C prepared by the present invention3N4The nano combined material of/ZnS
Material is than simple g-C3N4With ZnS, there is more preferable tribological property.
Claims (6)
1. a kind of g-C3N4The preparation method of/ZnS nano composite material, it is characterised in that comprise the steps：
Step 1, g-C3N4The preparation of dispersion liquid：
First preparation g-C3N4Powder, then by g-C3N4Powder is added in deionized water, supersound process, prepared g-C3N4Dispersion
Liquid；
Step 2, g-C3N4The preparation of/ZnS nano composite material：
First, successively zinc acetate, sodium sulfide, carbamide are added to step 1 gained g-C3N4In dispersion liquid, 5～10min of magnetic agitation,
Obtain mixed liquor；Subsequently, mixed liquor is moved into and reacts in hydrothermal reaction kettle of the politef for liner, after reaction terminates, natural
Room temperature is cooled to, product is collected by centrifugation, deionized water and dehydrated alcohol are washed to product, dry；Finally, g- is obtained
C3N4/ ZnS nano composite material.
2. a kind of g-C according to claim 13N4The preparation method of/ZnS nano composite material, it is characterised in that step 1
In, the g-C3N4The preparation method of powder is：With carbamide as raw material, 10g carbamide is placed in the corundum crucible with cover of 25mL,
It is transferred in chamber type electric resistance furnace, with 10～20 DEG C/min temperature programming to 550～600 DEG C, 2h is incubated, room temperature is naturally cooled to,
Obtain faint yellow g-C3N4Powder.
3. a kind of g-C according to claim 13N4The preparation method of/ZnS nano composite material, it is characterised in that step 2
In, the zinc acetate：The mol ratio of sodium sulfide is 1：1；In zinc element, sodium sulfide in the carbamide of the interpolation and zinc acetate
The ratio of element sulphur gross mass is 1：2～4, concentration of the carbamide in mixed liquor is 0.5～5mg/mL.
4. a kind of g-C according to claim 13N4The preparation method of/ZnS nano composite material, it is characterised in that step 2
In, it is 24h in 160～200 DEG C, response time that the reaction kettle for reaction condition is.
5. a kind of g-C according to claim 13N4The preparation method of/ZnS nano composite material, it is characterised in that step 2
In, the drying condition dries 12h for 60 DEG C.
6. a kind of g-C according to claim 13N4The preparation method of/ZnS nano composite material, it is characterised in that made
Standby g-C3N4In/ZnS nano composite material, g-C3N4Mass fraction be 50%～80%.
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| CN110586164A (en) * | 2019-09-29 | 2019-12-20 | 上海电力大学 | g-C3N4Preparation of/rGO/ZnS photocatalyst and application thereof in photoelectric chemical cathode protection |
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| CN110828191A (en) * | 2019-09-27 | 2020-02-21 | 西安交通大学 | Carbon nitride/graphene/nickel disulfide supercapacitor material with porous layered structure and preparation method thereof |
| CN113637200A (en) * | 2021-09-16 | 2021-11-12 | 南昌航空大学 | Composite dielectric film based on heterojunction double-interface layer nano material |
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| CN110586164A (en) * | 2019-09-29 | 2019-12-20 | 上海电力大学 | g-C3N4Preparation of/rGO/ZnS photocatalyst and application thereof in photoelectric chemical cathode protection |
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| CN113637200A (en) * | 2021-09-16 | 2021-11-12 | 南昌航空大学 | Composite dielectric film based on heterojunction double-interface layer nano material |
| CN113637200B (en) * | 2021-09-16 | 2022-03-15 | 南昌航空大学 | Composite dielectric film based on heterojunction double-interface layer nano material |
| CN114160177A (en) * | 2021-09-18 | 2022-03-11 | 鲁东大学 | Visible light response ZnS/C3N4Photocatalyst and preparation method thereof |
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