CN107233910A - The synthetic method of one species graphitic nitralloy carbon/stannous sulfide nano heterojunction - Google Patents
The synthetic method of one species graphitic nitralloy carbon/stannous sulfide nano heterojunction Download PDFInfo
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- 238000010189 synthetic method Methods 0.000 title claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 15
- 229910052799 carbon Inorganic materials 0.000 title abstract description 12
- DZXKSFDSPBRJPS-UHFFFAOYSA-N tin(2+);sulfide Chemical compound [S-2].[Sn+2] DZXKSFDSPBRJPS-UHFFFAOYSA-N 0.000 title abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 18
- 239000010431 corundum Substances 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004202 carbamide Substances 0.000 claims abstract description 13
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000002105 nanoparticle Substances 0.000 claims abstract description 6
- 238000011065 in-situ storage Methods 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 16
- 239000013049 sediment Substances 0.000 claims description 15
- 238000004140 cleaning Methods 0.000 claims description 9
- 239000011858 nanopowder Substances 0.000 claims description 9
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 9
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 239000012265 solid product Substances 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 2
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract 2
- 239000012467 final product Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 11
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 8
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 239000003125 aqueous solvent Substances 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 230000008901 benefit Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000010748 Photoabsorption Effects 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a species graphitic nitralloy carbon/stannous sulfide (g C3N4/ SnS) nano heterojunction synthetic method, comprise the following steps：1) a certain amount of urea is weighed to be put into corundum crucible；2) corundum crucible for filling urea is put into Muffle furnace to be calcined at a certain temperature, obtains g C3N4；3) a certain amount of SnCl is weighed2·2H2O is dissolved in deionized water, and a certain amount of g C are added after being sufficiently stirred for3N4, continue to stir；4) a certain amount of Na is weighed2S·9H2O is dissolved in deionized water, is added dropwise to g C3N4And SnCl2Suspension in, by stirring fully reaction；5) final product is obtained by separation, washing and after drying.Synthesis technique of the present invention is simple, g C3N4Growth in situ SnS nano-particles in nanometer sheet, the g C3N4/ SnS nano heterojunctions have meso-hole structure feature, there is larger specific surface area (80 90m2/ g), there is excellent photocatalysis performance under visible light conditions.
Description
Technical field
The present invention relates to a kind of chemical synthesis process of oxide semiconductor nano-powder, and in particular to a species graphite nitrogen
Change carbon/stannous sulfide (g-C3N4/ SnS) nano heterojunction synthetic method and product.
Background technology
Graphite phase carbon nitride (g-C3N4) it is a kind of organic polymer Nano semiconductor, metal ingredient is not contained, with similar
The laminated structure of graphene.With excellent chemical stability, semiconducting behavior, heat endurance, high-specific surface area, suitable energy level
Structure, makes it be widely used in photolysis water hydrogen gas, catalysis organic reaction and photocatalytic degradation organic matter etc. field, causes
The attention of many researchers.However, pure phase g-C3N4Band gap is wide, it is seen that light utilization ratio is low, and photo-generate electron-hole is to multiple
Close speed fast.Therefore in order to widen g-C3N4Optical absorption spectra scope, the present invention using with by the way of other semiconductors couplings to g-
C3N4It is modified.
The transfer of photo-generate electron-hole pair can be promoted by building heterojunction semiconductor, effectively reduction light induced electron and hole
Recombination probability, improves the separative efficiency of photo-generated carrier, increases its quantum efficiency, so as to improve photocatalysis performance.Semiconductor
The characteristics of hetero-junctions, can be by regulation constituent content to control its energy gap, can also make wide band gap semiconducter and arrowband
Gap semiconductor is combined to widen spectral response range, can improve solar energy utilization ratio.
The present invention chooses the different SnS and g-C of band gap width3N4System, SnS band gap magnitudes are smaller, have under visible light conditions
Good photo absorption performance, g-C is synthesized using thermal polymerization3N4Nano powder, then using precipitation method fabricated in situ nanometer g-C3N4/
SnS hetero-junctions, the product is expected to obtain excellent photocatalysis performance under visible light conditions, but g-C3N4The heterogeneous combinations of/SnS
Into method there is not yet related report.
The content of the invention
It is an object of the invention to provide a species graphitic nitralloy carbon/stannous sulfide (g-C3N4/ SnS) nano heterojunction
Synthetic method, this method technique is simple, easy to operate, and the product purity for reacting synthesis is high, and specific surface area is big, is urged with excellent light
Change performance, fill up class graphitic nitralloy carbon/stannous sulfide (g-C3N4/ SnS) nano composite material synthesis technical field blank.
The object of the invention to solve the technical problems is realized using following technical scheme.According to present invention proposition
A species graphitic nitralloy carbon/stannous sulfide (g-C3N4/ SnS) nano heterojunction synthetic method, comprise the following steps：
(1) a certain amount of urea is weighed, is placed on after being ground in agate mortar and is transferred in corundum crucible；
(2) it will be put into Muffle furnace and calcine after the corundum crucible capping in step (1), be subsequently cooled to room temperature, take out, receive
Collect product g-C3N4；
(3) by SnCl2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred for2Solution, resulting solution
Middle Sn2+Concentration be 0.2mol/L, in SnCl2The g-C that step (2) is prepared is added in solution3N4Nano powder, is sufficiently stirred for mixing
Close uniform, be designated as suspension A；
(4) by Na2S·9H2O is soluble in water, makes S in resulting solution2-Concentration be 0.2mol/L, then by Na2S solution
Added with 0.5ml/min drop rates in suspension A prepared by step (3), 2h is stirred after completion of dropwise addition makes its reaction abundant；Its
In, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and be centrifuged, solid is taken after centrifugation
Sediment, is cleaned to obtained solid sediment, then the solid product obtained after cleaning is put into drying box, in 50-
10-12h is dried at a temperature of 70 DEG C, g-C is obtained3N4/ SnS nano heterojunctions.
The object of the invention to solve the technical problems can be also applied to the following technical measures to achieve further.
A foregoing species graphitic nitralloy carbon/stannous sulfide (g-C3N4/ SnS) nano heterojunction synthetic method, wherein,
A certain amount of urea described in step (1) refers to that compactedness of the urea in corundum crucible is (50-60) %.
A foregoing species graphitic nitralloy carbon/stannous sulfide (g-C3N4/ SnS) nano heterojunction synthetic method, wherein,
Holding temperature is 570-600 DEG C when being calcined in step (2), and heating rate is 3-5 DEG C/min, and soaking time is 3-4h.
A foregoing species graphitic nitralloy carbon/stannous sulfide (g-C3N4/ SnS) nano heterojunction synthetic method, wherein,
Cleaning method described in step (5) is：Obtained solid sediment is replaced using deionized water and absolute ethyl alcohol successively
Washing 3-5 times.
A foregoing species graphitic nitralloy carbon/stannous sulfide (g-C3N4/ SnS) nano heterojunction synthetic method, wherein,
G-C obtained by step (5)3N4/ SnS nano heterojunctions include g-C3N4With SnS two-phases, wherein SnS mass fraction is (1-
10) %.
A foregoing species graphitic nitralloy carbon/stannous sulfide (g-C3N4/ SnS) nano heterojunction synthetic method, wherein,
G-C in final gained synthetic product3N4For laminated structure, its thickness is 20-30nm, g-C3N4Surface in situ growth has SnS nanometers
Particle, a diameter of 10-20nm of SnS nano particles.
The present invention has clear advantage and beneficial effect compared with prior art, by above-mentioned technical proposal, the present invention
A kind of g-C3N4The synthetic method of/SnS nano heterojunctions can reach suitable technological progress and practicality, and with industry
Extensive value, its at least have following advantages：
1st, g-C is synthesized using two-step method3N4/ SnS nano heterojunctions, synthesis technique used is simple, easy to operate, and reaction is closed
Into product purity it is high.
2nd, g-C prepared by this method3N4/ SnS nano heterojunctions, with meso-hole structure feature and larger surface area
(80-90m2/ g), photocatalytic degradation experiment is carried out to methylene blue (MB) solution under visible ray (xenon lamp) irradiation, it is shown that excellent
Different photocatalysis performance.
In summary, a kind of g-C of the invention3N4The synthetic method of/SnS nano heterojunctions technically has significant progress,
And be really a new and innovative, progressive, practical new design with obvious good effect.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, and in order to allow the above and other objects, features and advantages of the present invention can
Become apparent, below especially exemplified by preferred embodiment, and coordinate accompanying drawing, describe in detail as follows.
Brief description of the drawings
It is g-C made from embodiment 1 to scheme (1)3N4/ SnS XRD；
It is g-C made from embodiment 1 to scheme (2)3N4/ SnS TEM figures；
It is g-C made from embodiment 1 to scheme (3)3N4The concentration curve figure of/SnS degradation of methylene blue solution；
It is g-C made from embodiment 1 to scheme (4)3N4/ SnS and g-C3N4Photocatalysis results contrast under the conditions of same test
Figure；
Embodiment
Further to illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below in conjunction with
Accompanying drawing and preferred embodiment, to according to a kind of g-C proposed by the present invention3N4The synthetic method of/SnS nano heterojunctions, it is specific real
Mode, structure, feature and its effect are applied, is described in detail as after.
Embodiment 1：
(1) a certain amount of urea is weighed, is placed on after being ground in agate mortar and is transferred in corundum crucible；
(2) it will be placed in Muffle furnace and calcine after the corundum crucible capping in step (1), heating rate is 3 DEG C/min,
Holding temperature is 600 DEG C, and soaking time is 4h, is cooled to after room temperature and takes out, collects product g-C3N4；
(3) a certain amount of SnCl is weighed2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred for2Solution,
Sn in resulting solution2+Concentration be 0.2mol/L, in SnCl2A certain amount of g-C is added in solution3N4Nano powder, is sufficiently stirred for mixing
Close uniform, be designated as suspension A；
(4) weigh a certain amount of vulcanized sodium to be dissolved in aqueous solvent, make S in resulting solution2-Concentration be 0.2 mol/L, so
Afterwards by Na2S solution is added in the suspension A prepared to step (3) with 0.5ml/min drop rates, and 2h is stirred after completion of dropwise addition
Make its reaction abundant；Wherein, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and be centrifuged, take solid sediment, it
Afterwards, alternately washing 3 times, then will be obtained after cleaning are carried out using deionized water and absolute ethyl alcohol successively to obtained solid sediment
Solid product be put into drying box, at a temperature of 60 DEG C dry 10h, obtain g-C3N4/ SnS nano heterojunctions.
Gained g-C3N4G-C in/SnS nano heterojunctions3N4Mass fraction be 97%, SnS mass fraction be 3%.
The g-C that the present embodiment is obtained3N4/ SnS carries out XRD and TEM and tested, test result as depicted in figs. 1 and 2, by scheming
Understand：G-C is included in synthetic product3N4With SnS two-phases, g-C3N4For laminated structure, its thickness is 20-30nm or so, its surface
Growth in situ has SnS nano particles；A diameter of 10-20nm of SnS nano particles.
Photocatalysis performance test is carried out to synthetic product, 0.05g g-C is taken respectively3N4And this implementation (as a control group)
The nanometer, composite semiconductor g-C of example synthesis3N4/ SnS (being used as test group) is as photochemical catalyst, with methylene blue (MB) for target
Degradation product (concentration is 7mg/L), the equal 50ml of volume, from 150W xenon lamp as light source, distance of the sample away from fluorescent tube is
15cm, carries out photocatalytic degradation experiment.As a result as shown in figure 3, g-C after illumination 30min3N4/ SnS degrades to methylene blue solution
Almost completely, Fig. 4 shows, by 30min illumination, g-C3N4Degradable MB degradeds 62% or so, and g-C3N4The degradable MB of/SnS
Degraded 95%, contrast degradation results can show that its photocatalysis performance can be significantly improved by building composite semiconductor.
Embodiment 2：
(1) a certain amount of urea is weighed, is placed on after being ground in agate mortar and is transferred in corundum crucible；
(2) it will place in Muffle furnace and calcine after the corundum crucible capping in step (1), heating rate is 4 DEG C/min, is protected
Temperature is 570 DEG C, and soaking time is 3h, is cooled to after room temperature and takes out, collects product g-C3N4；
(3) a certain amount of SnCl is weighed2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred for2Solution,
Sn in resulting solution2+Concentration be 0.2mol/L, in SnCl2The g-C that a certain amount of step (2) is prepared is added in solution3N4
Nano powder, is thoroughly mixed uniform；It is designated as suspension A；
(4) weigh a certain amount of vulcanized sodium to be dissolved in aqueous solvent, make S in resulting solution2-Concentration be 0.2 mol/L, so
Afterwards by Na2S solution is added in the suspension A prepared to step (3) with 0.5ml/min drop rates, and 2h is stirred after completion of dropwise addition
Make its reaction abundant；Wherein, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and be centrifuged, take solid sediment, it
Afterwards, alternately washing 5 times, then will be obtained after cleaning are carried out using deionized water and absolute ethyl alcohol successively to obtained solid sediment
Solid product be put into drying box, under the conditions of 70 DEG C dry 10h, obtain g-C3N4/ SnS nano heterojunctions.
Gained g-C3N4G-C in/SnS nano heterojunctions3N4Mass fraction be 95%, SnS mass fraction be 5%.
Embodiment 3：
(1) a certain amount of urea is weighed, is placed on after being ground in agate mortar and is transferred in corundum crucible；
(2) it will place in Muffle furnace and calcine after the corundum crucible capping in step (1), heating rate is 3 DEG C/min, is protected
Temperature is 580 DEG C, and soaking time is 3h, is cooled to after room temperature and takes out, collects product g-C3N4；
(3) a certain amount of SnCl is weighed2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred for2Solution,
Sn in resulting solution2+Concentration be 0.2mol/L, in SnCl2The g-C that a certain amount of step (2) is prepared is added in solution3N4
Nano powder, is thoroughly mixed uniform；It is designated as suspension A；
(4) weigh a certain amount of vulcanized sodium to be dissolved in aqueous solvent, make S in resulting solution2-Concentration be 0.2 mol/L, so
Afterwards by Na2S solution is added in the suspension A prepared to step (3) with 0.5ml/min drop rates, and 2h is stirred after completion of dropwise addition
Make its reaction abundant；Wherein, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and be centrifuged, take solid sediment, it
Afterwards, alternately washing 3 times, then will be obtained after cleaning are carried out using deionized water and absolute ethyl alcohol successively to obtained solid sediment
Solid product be put into drying box, under the conditions of 70 DEG C dry 12h, obtain g-C3N4/ SnS nano heterojunctions.
Gained g-C3N4G-C in/SnS nano heterojunctions3N4Mass fraction be 90%, SnS mass fraction be 10%.
Embodiment 4：
(1) a certain amount of urea is weighed, is placed on after being ground in agate mortar and is transferred in corundum crucible；
(2) it will place in Muffle furnace and calcine after the corundum crucible capping in step (1), heating rate is 5 DEG C/min, is protected
Temperature is 600 DEG C, and soaking time is 4h, is cooled to after room temperature and takes out, collects product g-C3N4；
(3) a certain amount of SnCl is weighed2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred for2Solution,
Sn in resulting solution2+Concentration be 0.2mol/L, in SnCl2The g-C that a certain amount of step (2) is prepared is added in solution3N4
Nano powder, is thoroughly mixed uniform；It is designated as suspension A；
(4) weigh a certain amount of vulcanized sodium to be dissolved in aqueous solvent, make S in resulting solution2-Concentration be 0.2 mol/L, so
Afterwards by Na2S solution is added in the suspension A prepared to step (3) with 0.5ml/min drop rates, and 2h is stirred after completion of dropwise addition
Make its reaction abundant；Wherein, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and be centrifuged, take solid sediment, it
Afterwards, alternately washing 4 times, then will be obtained after cleaning are carried out using deionized water and absolute ethyl alcohol successively to obtained solid sediment
Solid product be put into drying box, under the conditions of 65 DEG C dry 12h, obtain g-C3N4/ SnS nano heterojunctions.
Gained g-C3N4G-C in/SnS nano heterojunctions3N4Mass fraction be 94%, SnS mass fraction be 6%.
Embodiment 5：
(1) a certain amount of urea is weighed, is placed on after being ground in agate mortar and is transferred in corundum crucible；
(2) it will place in Muffle furnace and calcine after the corundum crucible capping in step (1), heating rate is 4 DEG C/min, is protected
Temperature is 590 DEG C, and soaking time is 4h, is cooled to after room temperature and takes out, collects product g-C3N4；
(3) a certain amount of SnCl is weighed2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred for2Solution,
Sn in resulting solution2+Concentration be 0.2mol/L, in SnCl2The g-C that a certain amount of step (2) is prepared is added in solution3N4
Nano powder, is thoroughly mixed uniform；It is designated as suspension A；
(4) weigh a certain amount of vulcanized sodium to be dissolved in aqueous solvent, make S in resulting solution2-Concentration be 0.2 mol/L, so
Afterwards by Na2S solution is added in the suspension A prepared to step (3) with 0.5ml/min drop rates, and 2h is stirred after completion of dropwise addition
Make its reaction abundant；Wherein, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and be centrifuged, take solid sediment, it
Afterwards, obtained solid sediment is alternately washed 4 times using deionized water and absolute ethyl alcohol progress successively, then will be obtained after cleaning
To solid product be put into drying box, under the conditions of 60 DEG C dry 12h, obtain g-C3N4/ SnS nano heterojunctions.
Gained g-C3N4G-C in/SnS nano heterojunctions3N4Mass fraction be 92%, SnS mass fraction be 8%.
The above described is only a preferred embodiment of the present invention, any formal limitation not is made to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any to be familiar with this professional technology people
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit according to the present invention
Any simple modification, equivalent variations and the modification made to above example, in the range of still falling within technical solution of the present invention.
Claims (6)
1. a kind of g-C3N4The synthetic method of/SnS nano heterojunctions, it is characterised in that comprise the following steps：
(1) a certain amount of urea is weighed, is placed on after being ground in agate mortar and is transferred in corundum crucible；
(2) it will be put into Muffle furnace and calcine after the corundum crucible capping in step (1), be subsequently cooled to room temperature, take out, collect production
Thing g-C3N4；
(3) by SnCl2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred for2Sn in solution, resulting solution2+
Concentration be 0.2mol/L, in SnCl2The g-C that step (2) is prepared is added in solution3N4Nano powder, is thoroughly mixed
It is even, it is designated as suspension A；
(4) by Na2S·9H2O is soluble in water, makes S in resulting solution2-Concentration be 0.2mol/L, then by Na2S solution with
0.5ml/min drop rates are added in suspension A prepared by step (3), and 2h is stirred after completion of dropwise addition makes its reaction abundant；Its
In, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and be centrifuged, take solid to precipitate after centrifugation
Thing, is cleaned to obtained solid sediment, then the solid product obtained after cleaning is put into drying box, at 50-70 DEG C
At a temperature of dry 10-12h, obtain g-C3N4/ SnS nano heterojunctions.
2. a kind of g-C according to claim 13N4The synthetic method of/SnS nano heterojunctions, it is characterised in that step (1)
Described a certain amount of urea refers to that compactedness of the urea in corundum crucible is (50-60) %.
3. a kind of g-C according to claim 13N4The synthetic method of/SnS nano heterojunctions, it is characterised in that step (2)
Holding temperature is 570-600 DEG C during middle calcining, and heating rate is 3-5 DEG C/min, and soaking time is 3-4h.
4. a kind of g-C according to claim 13N4The synthetic method of/SnS nano heterojunctions, it is characterised in that step (5)
Described cleaning method is：Alternately washing 3-5 is carried out to obtained solid sediment using deionized water and absolute ethyl alcohol successively
It is secondary.
5. a kind of g-C according to claim 13N4The synthetic method of/SnS nano heterojunctions, it is characterised in that step (5)
Gained g-C3N4/ SnS nano heterojunctions include g-C3N4With SnS two-phases, wherein SnS mass fraction is (1-10) %.
6. a kind of g-C according to claim 13N4The synthetic method of/SnS nano heterojunctions, it is characterised in that final gained
G-C in synthetic product3N4For laminated structure, its thickness is 20-30nm, g-C3N4Surface in situ growth has SnS nano particles, SnS
A diameter of 10-20nm of nano particle.
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| Publication number | Priority date | Publication date | Assignee | Title |
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