CN106430288B - A kind of g C3N4The preparation method of/ZnS nanocomposites - Google Patents
A kind of g C3N4The preparation method of/ZnS nanocomposites Download PDFInfo
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- C01G9/08—Sulfides
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- 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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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/061—Carbides; Hydrides; Nitrides
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/065—Sulfides; Selenides; Tellurides
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- 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 present invention provides a kind of g C3N4The preparation method of/ZnS nanocomposites, including：1、g‑C3N4The preparation of dispersion liquid：Head prepares g C3N4Powder, then by g C3N4Powder is added in deionized water, is ultrasonically treated, and g C are made3N4Dispersion liquid；2、g‑C3N4The preparation of/ZnS nanocomposites：Zinc acetate, vulcanized sodium, urea are added to step 1 gained g C successively3N4In dispersion liquid, 5~10min of magnetic agitation, obtains mixed liquor；Mixed liquor is moved into polytetrafluoroethylene (PTFE) to be reacted in the hydrothermal reaction kettle of liner, after reaction, cooled to room temperature, is collected by centrifugation product, and product is washed with deionized water and absolute ethyl alcohol, dry；Finally, g C are obtained3N4/ ZnS nanocomposites.Simple production process of the present invention is easily-controllable, and reaction condition is gentle, yield height and favorable reproducibility, prepares the g C of gained3N4/ ZnS nano-complex grain sizes are uniform, good dispersion, can be applied to the fields such as lube oil additive, photoelectric material, hydrogen storage, photocatalysis.
Description
Technical field
The invention belongs to field of nanocomposite materials, specifically discloses a kind of g-C3N4The preparation of/ZnS nanocomposites
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, these materials are widely used as lithium-ion electric
Pond electrode, lube oil additive, new catalyst and thermoelectric material etc., wherein, ZnS as transition metal chalcogenide one
Member, is II-VI races wide bandgap semiconductor compound-material, its Emission in Cubic energy gap is 3.7eV, and hexagonal phase energy gap is
3.8eV.As a kind of semi-conducting material, ZnS is in flat-panel monitor, electroluminescent, device for non-linear optical, cathode-ray hair
Light, light emitting diode, field-effect transistor, solar cell, dielectric filter, infrared window material, dyestuff, photocatalysis, sensor
And laser, solid lubrication etc. suffers from being widely applied.When the particle diameter of ZnS particles is less than the Bohr radius of its exciton,
It can show obvious quantum size effect, and its photoelectricity, frictional behaviour also can with the change of size and pattern and
Change.Therefore, the preparation of ZnS and performance study cause the broad interest of domestic and foreign scholars.So far, lot of domestic and foreign section
Group is ground successfully to synthesize ZnS nanometer rods, nano wire by different synthetic methods, nanometer sheet, nanobelt, 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 are with sp2Hydridization formed height from
The pi-conjugated system in domain.g-C3N4Not only with the deriving from a wealth of sources of polymeric material, the relatively low advantage of price, but also its excellent light is urged
Changing performance can also 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, there is preferable photocatalysis performance, therefore is widely used as photochemical catalyst, such as
Photocatalysis degradation organic contaminant, photocatalysis liberation of hydrogen and photocatalysis organic synthesis etc..In addition, researcher employs pattern tune
The strategies such as control, element doping, semiconductors coupling, effectively increase its photocatalytic activity.Recent studies have shown that g-C3N4It can increase
Original performance of strong composite material, therefore g-C3N4Based nano composite material lithium electricity, fuel sensitized cells, ultracapacitor and
The fields such as lubrication have potential application prospect.g-C3N4Although cannot be compared with graphene in intensity, it can be gentle
Under conditions of carried out by a series of predecessor (melamine etc.) of carbon containing rich 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,
Photochemical catalyst, gas storage etc. 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 domestic and foreign scholars and researcher to this with unlimited potentiality
The tireless exploration of new material.
Based on g-C3N4, ZnS good characteristic, g-C3N4/ ZnS nanocomposites can show its opposite homogenous material
More comprehensive, excellent performance.For nanocomposite, research concentrates on graphene-based nano combined material mostly at present
Material, as graphene/molybdenum disulfide nano answers material, 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 materials, and in fields such as tribology, catalysis, lithium electricity
With good development prospect.
The 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 materials, to improve sulphur
Change the performances such as electricity, calorifics, catalysis and the tribology of zinc and extend its application field.
The present invention is achieved through the following technical solutions：
A kind of g-C3N4The preparation method of/ZnS nanocomposites, includes the following steps：
Step 1, g-C3N4The preparation of dispersion liquid：
Head prepares g-C3N4Powder, then by g-C3N4Powder is added in deionized water, is ultrasonically treated, and g-C is made3N4Point
Dispersion liquid；
Step 2, g-C3N4The preparation of/ZnS nanocomposites：
First, zinc acetate, vulcanized sodium, urea are added to step 1 gained g-C successively3N4In dispersion liquid, magnetic agitation 5~
10min, obtains mixed liquor；Then, mixed liquor is moved into polytetrafluoroethylene (PTFE) to be reacted in the hydrothermal reaction kettle of liner, reaction terminates
Afterwards, cooled to room temperature, is collected by centrifugation product, and product is washed with deionized water and absolute ethyl alcohol, dry；Finally,
Obtain g-C3N4/ ZnS nanocomposites.
In step 1, the g-C3N4The preparation method of powder is：Using urea as raw material, 10g urea 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 programmings to 550~600 DEG C, keeps the temperature 2h, from
Room temperature so is cooled to, obtains faint yellow g-C3N4Powder.
In step 2, the zinc acetate：The molar ratio of vulcanized sodium is 1：1；Zinc member in the urea and zinc acetate of the addition
The ratio between element sulphur gross mass in element, vulcanized sodium is 1：2~4, concentration of the urea in mixed liquor is 0.5~5mg/mL.
In step 2, reaction condition is 160~200 DEG C in the reaction kettle, reaction time 24h.
In step 2, the drying condition is 60 DEG C of dry 12h.
Prepared g-C3N4In/ZnS nanocomposites, 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, yield height and favorable reproducibility, system
The g-C of standby gained3N4/ ZnS nano-complex grain sizes are uniform, good dispersion, can be applied to lube oil additive, photoelectricity material
The fields such as material, hydrogen storage, photocatalysis, have a good application prospect.
Brief description of the drawings
Fig. 1 is the g-C that example 1 synthesizes3N4SEM figure.
Fig. 2 is the g-C synthesized in example 23N4With g-C3N4The XRD diagram of/ZnS nanocomposites.
Fig. 3 is the g-C that example 3 synthesizes3N4The SEM figures of/ZnS nanocomposite difference up-sizings.
Fig. 4 is the g-C that example 3 synthesizes3N4/ ZnS nanocomposites EDS schemes.
Fig. 5 is the g-C that example 4 synthesizes3N4/ ZnS nanocomposites TEM schemes.
Fig. 6 is the g-C synthesized in example 23N4The friction coefficient figure of/ZnS nanocomposites.
Embodiment
Urea chemical formula used in the present invention is CO (NH2)2, molecular weight 60.06；Zinc source is zinc acetate, and chemical formula is
C4H6O4Zn·2H2O, molecular weight 219.51；Sulphur source is vulcanized sodium, chemical formula Na2S·9H2O, molecular weight 240.18.
Embodiment 1：
(1)g-C3N4Preparation：
Using urea as raw material, 10g urea is placed in the corundum crucible with cover of 25mL, is transferred in chamber type electric resistance furnace, risen
For temperature to 550 DEG C, programming rate is 10 DEG C/min, keeps the temperature 2h, naturally cools to room temperature, obtain faint yellow g-C3N4Powder.
(2)g-C3N4The preparation of/ZnS nanocomposites：
Weigh obtained g-C in step (1)3N4Powder 0.16g (50%) is added in 40mL deionized waters, is ultrasonically treated
30min, is made the dispersion liquid that concentration is 4mg/mL；Then, according to zinc acetate：Vulcanized sodium=1：1 molar ratio weighs zinc acetate
0.3604g, vulcanized sodium 0.3944g, are according to the ratio between the element sulphur gross mass of urea with the Zn-ef ficiency in zinc acetate, in vulcanized sodium
1：2 weigh urea 0.08g, are added to g-C3N4In dispersion liquid, 5~10min of magnetic agitation, obtains mixed liquor；Finally, by mixed liquor
Polytetrafluoroethylene (PTFE) is moved into as in the hydrothermal reaction kettle of liner, the hydro-thermal 24h under conditions of 160 DEG C, after cooled to room temperature from
The heart collects product, and product is washed with deionized water and absolute ethyl alcohol, and finally dry 12h obtains g-C at 60 DEG C3N4/
ZnS nanocomposites.
The SEM figures of Fig. 1 are it can be seen that the g-C prepared3N4Lamellar structure with class graphene, thickness is within 100nm.
Embodiment 2：
(1)g-C3N4Preparation：
Using urea as raw material, 10g urea is placed in the corundum crucible with cover of 25mL, is transferred in chamber type electric resistance furnace, risen
For temperature to 570 DEG C, programming rate is 15 DEG C/min, keeps the temperature 2h, naturally cools to room temperature, obtain faint yellow g-C3N4Powder.
(2)g-C3N4The preparation of/ZnS nanocomposites：
Weigh obtained g-C in step (1)3N4Powder 0.24g (60%) is added in 40mL deionized waters, is ultrasonically treated
30min, is made the dispersion liquid that concentration is 6mg/mL；Then, according to zinc acetate：Vulcanized sodium=1：1 molar ratio weighs zinc acetate
0.3604g, vulcanized sodium 0.3944g, are according to the ratio between the element sulphur gross mass of urea with the Zn-ef ficiency in zinc acetate, in vulcanized sodium
1：4 weigh urea 0.04g, are added to g-C3N4In dispersion liquid, 5~10min of magnetic agitation, obtains mixed liquor；Finally, by mixed liquor
Polytetrafluoroethylene (PTFE) is moved into as in the hydrothermal reaction kettle of liner, the hydro-thermal 24h under conditions of 180 DEG C, after cooled to room temperature from
The heart collects product, and product is washed with deionized water and absolute ethyl alcohol, and finally dry 12h obtains g-C at 60 DEG C3N4/
ZnS nanocomposites.
The XRD spectrum of Fig. 2 can be seen that the g-C of synthesis3N4With higher purity, simultaneously synthesizing nanocomposite
Collection of illustrative plates in, ZnS has higher crystallinity, and the g-C that still withs a hook at the end3N4Peak, illustrate that two kinds of materials exist, preliminary explanation
g-C3N4The successful synthesis of/ZnS.
Embodiment 3：
(1)g-C3N4Preparation：
Using urea as raw material, 10g urea is placed in the corundum crucible with cover of 25mL, is transferred in chamber type electric resistance furnace, risen
For temperature to 580 DEG C, programming rate is 15 DEG C/min, keeps the temperature 2h, naturally cools to room temperature, obtain faint yellow g-C3N4Powder.
(2)g-C3N4The preparation of/ZnS nanocomposites：
Weigh obtained g-C in step (1)3N4Powder 0.32g (70%) is added in 40mL deionized waters, is ultrasonically treated
30min, is made the dispersion liquid that concentration is 8mg/mL；Then, according to zinc acetate：Vulcanized sodium=1：1 molar ratio weighs zinc acetate
0.3090g, vulcanized sodium 0.3380g, are according to the ratio between the element sulphur gross mass of urea with the Zn-ef ficiency in zinc acetate, in vulcanized sodium
1：2 weigh urea 0.069g, are added to g-C3N4In dispersion liquid, 5~10min of magnetic agitation, obtains mixed liquor；Finally, by mixed liquor
Polytetrafluoroethylene (PTFE) is moved into as in the hydrothermal reaction kettle of liner, the hydro-thermal 24h under conditions of 180 DEG C, after cooled to room temperature from
The heart collects product, and product is washed with deionized water and absolute ethyl alcohol, and finally dry 12h obtains g-C at 60 DEG C3N4/
ZnS nanocomposites.
The SEM figures of Fig. 3 are it can be seen that the g-C prepared3N4/ ZnS has ideal 2D/3D heterojunction structures, block shape
G-C3N4Surface is thickly dotted to be loaded with a large amount of ZnS nano particles, and particle 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, without other any miscellaneous
Prime element.
Embodiment 4：
(1)g-C3N4Preparation：
Using urea as raw material, 10g urea is placed in the corundum crucible with cover of 25mL, is transferred in chamber type electric resistance furnace, risen
For temperature to 600 DEG C, programming rate is 20 DEG C/min, keeps the temperature 2h, naturally cools to room temperature, obtain faint yellow g-C3N4Powder.
(2)g-C3N4The preparation of/ZnS nanocomposites：
Weigh obtained g-C in step (1)3N4Powder 0.32g (80%) is added in 40mL deionized waters, is ultrasonically treated
30min, is made the dispersion liquid that concentration is 8mg/mL；Then, according to zinc acetate：Vulcanized sodium=1：1 molar ratio weighs zinc acetate
0.1802g, vulcanized sodium 0.1972g, are according to the ratio between the element sulphur gross mass of urea with the Zn-ef ficiency in zinc acetate, in vulcanized sodium
1：4 weigh urea 0.02g, are added to g-C3N4In dispersion liquid, 5~10min of magnetic agitation, obtains mixed liquor；Finally, by mixed liquor
Polytetrafluoroethylene (PTFE) is moved into as in the hydrothermal reaction kettle of liner, the hydro-thermal 24h under conditions of 200 DEG C, after cooled to room temperature from
The heart collects product, and product is washed with deionized water and absolute ethyl alcohol, and finally dry 12h obtains g-C at 60 DEG C3N4/
ZnS nanocomposites.
The TEM figures of Fig. 5 further can clearly find out the g-C of preparation3N4/ ZnS nanocomposites have ideal
Hetero-junctions pattern, g-C3N4Nanometer sheet surface appendix has ZnS nano-particles, and particle is in spherical, and particle diameter is in 20-30nm.
Embodiment 5：
By g-C prepared in example 23N4/ ZnS nanometers of self-lubricating composite, which is added in lubricating base oils, to rub
Wipe experiment, and with pure base oil, g-C3N4, zinc sulphide compares.Frictional experiment is tested in CETR UMT-2 multifunction friction wears
Carried out on machine.Using ball-disc type contact, a diameter of 4mm of stainless steel ball.Experiment load is 10N, speed of experiment 100r/min
(radius of gyration r=3mm).By prepared g-C3N4/ZnS、g-C3N4With ZnS basis is added according to certain mass percent
In oily HVI750, with being not added with the base oil HVI750 of the lubricant ultrasonic disperse 2h in ultrasonic washing instrument.Frictional experiment is surveyed
Test result is as shown in fig. 6, as seen from the figure, g-C3N4With the g-C prepared by ZnS and the present invention3N4/ ZnS nanocomposites
Obvious antifriction effect, but the g-C prepared by the present invention are respectively provided with when as lube oil additive3N4The nano combined materials of/ZnS
Material is than simple g-C3N4There is more preferable tribological property with ZnS.
Claims (5)
- A kind of 1. g-C3N4The preparation method of/ZnS nanocomposites, it is characterised in that include the following steps：Step 1, g-C3N4The preparation of dispersion liquid：Head prepares g-C3N4Powder, then by g-C3N4Powder is added in deionized water, is ultrasonically treated, and g-C is made3N4It is scattered Liquid；Step 2, g-C3N4The preparation of/ZnS nanocomposites：First, zinc acetate, vulcanized sodium, urea are added to step 1 gained g-C successively3N4In dispersion liquid, 5 ~ 10min of magnetic agitation, Obtain mixed liquor；Then, mixed liquor is moved into polytetrafluoroethylene (PTFE) to be reacted in the hydrothermal reaction kettle of liner, it is after reaction, natural It is cooled to room temperature, product is collected by centrifugation, product is washed with deionized water and absolute ethyl alcohol, it is dry；Finally, g- is obtained C3N4/ ZnS nanocomposites；The element sulphur gross mass in Zn-ef ficiency, vulcanized sodium in the urea and zinc acetate of the addition it Than for 1：2 ~ 4, concentration of the urea in mixed liquor is 0.5 ~ 5mg/mL；Prepared g-C3N4/ ZnS nanocomposites In, g-C3N4Mass fraction be 50% ~ 80%.
- A kind of 2. g-C according to claim 13N4The preparation method of/ZnS nanocomposites, it is characterised in that step 1 In, the g-C3N4The preparation method of powder is：Using urea as raw material, 10g urea 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 programmings to 550 ~ 600 DEG C, keeps the temperature 2h, naturally cool to room temperature, obtain To faint yellow g-C3N4Powder.
- A kind of 3. g-C according to claim 13N4The preparation method of/ZnS nanocomposites, it is characterised in that step 2 In, the zinc acetate：The molar ratio of vulcanized sodium is 1：1.
- A kind of 4. g-C according to claim 13N4The preparation method of/ZnS nanocomposites, it is characterised in that step 2 In, reaction condition is 160 ~ 200 DEG C in the reaction kettle, reaction time 24h.
- A kind of 5. g-C according to claim 13N4The preparation method of/ZnS nanocomposites, it is characterised in that step 2 In, the drying condition is 60 DEG C of dry 12h.
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| CN102145915B (en) * | 2011-03-04 | 2012-08-29 | 北京化工大学 | Method for synthetizing ZnS/CdS nano rod by controlling oxygen content in thermal process of solvent |
| CN102249289A (en) * | 2011-05-27 | 2011-11-23 | 新疆大学 | Method for preparing spiauterite ZnS fine nanorod with solvothermal method |
| CN104108742A (en) * | 2013-04-19 | 2014-10-22 | 李孝凤 | ZnS/SnS composite material powder synthesized by utilizing high-pressure solvothermal |
| CN105728012A (en) * | 2016-02-17 | 2016-07-06 | 常州市庆发工业气体有限公司 | Preparation method of carbon nitride imvite composite photocatalyst carrier |
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