CN108579767A - It is grown on the Sb of graphene surface2S3Nanometer sheet and its preparation method and application - Google Patents
It is grown on the Sb of graphene surface2S3Nanometer sheet and its preparation method and application Download PDFInfo
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- CN108579767A CN108579767A CN201810417304.6A CN201810417304A CN108579767A CN 108579767 A CN108579767 A CN 108579767A CN 201810417304 A CN201810417304 A CN 201810417304A CN 108579767 A CN108579767 A CN 108579767A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 6
- 239000010439 graphite Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 5
- 230000008520 organization Effects 0.000 claims abstract description 5
- 239000002356 single layer Substances 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000004108 freeze drying Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 12
- 229910052959 stibnite Inorganic materials 0.000 claims description 10
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 235000013878 L-cysteine Nutrition 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000004201 L-cysteine Substances 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 11
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 238000007605 air drying Methods 0.000 abstract description 3
- 238000010189 synthetic method Methods 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 235000018417 cysteine Nutrition 0.000 abstract 1
- 150000001945 cysteines Chemical class 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- 230000005355 Hall effect Effects 0.000 description 1
- 150000008538 L-cysteines Chemical class 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical class OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- IHBMMJGTJFPEQY-UHFFFAOYSA-N sulfanylidene(sulfanylidenestibanylsulfanyl)stibane Chemical compound S=[Sb]S[Sb]=S IHBMMJGTJFPEQY-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B01J35/33—
-
- B01J35/39—
-
- B01J35/61—
-
- B01J35/647—
Abstract
The invention belongs to the preparations of meso-porous nano material, are grown on the Sb of graphene surface2S3Nanometer sheet and its preparation method and application has sheet Sb for ultra-thin mono-layer graphite surface growth2S3, there is mesoporous hierarchical organization, by SbCl3It is dissolved in ethylene glycol solution, dodecyl sodium sulfate is added, the Graphene powder of freeze-drying is dissolved in ethylene glycol solution, be added in reaction system, L cysteines are added into mixed liquor, NaOH solution adds dropwise；Isothermal reaction is for 24 hours under 150 DEG C of hydrothermal conditions；Product uses deionized water and washes of absolute alcohol, natural air drying respectively, and under an ar atmosphere, 200 DEG C of burning 3h obtain target product.It is an advantage of the invention that：The Sb of preparation2S3/ graphene composite structure is the sheet Sb of ultra-thin mono-layer graphite surface growth2S3, there is mesoporous hierarchical organization, there is higher specific surface area, larger porosity；Synthetic method craft is simple, of low cost, reaction process is mild, and obtained product pattern is good, has application prospect in photoelectric properties.
Description
Technical field
The invention belongs to the preparations of meso-porous nano material, are grown on the Sb of graphene surface2S3Nanometer sheet and preparation method thereof
And purposes.
Background technology
Graphene has outstanding physics and electrical properties, such as high-specific surface area, high conductivity, high mechanical strength, is easy to
Modification and large-scale production etc..Graphene is zero gap semiconductor, there is unique carrier properties, is Relativistic Mechanics phenomenon
Research provide an important channel；The resistance very little that electronics transmits in graphene does not have when sub-micron distance is mobile
Scattering has good electronic transport property；The distinctive band structure of graphene makes hole and electronics be separated from each other, and results in new
The generation of electronics conduction phenomenon, such as quantum Interference, irregular quantum hall effect, this makes graphene at many aspects
Has the characteristic for surmounting current material；
Sb2S3It is the main component of stibnite, earth's crust rich content, material is cheaply nontoxic, and is inhaled with sunlight is suitable for
The band gap width and absorptivity of receipts are hopeful to be applied to prepare photoelectrocatalysimaterial material very much.Sb2S3Belong to rhombic system, space group
For Pbnm62, have high concentration anisotropy, band gap width 1.5-2.2eV big to the response range of visible light.And Sb2S3
The absorption coefficient of light be up to 105cm-1, it is highly suitable as light absorbing material.Sb2S3Crystal is a kind of with high anisotropy
Layer structure semi-conducting material, readily along c-axis direction grow or rupture, to form nanometer rods, nano wire, nanotube etc.
One-dimensional nano structure.Few precedents that flake nano structure is prepared by straightforward procedure.
Invention content
The present invention is to be based on background above, provides a kind of synthesizing graphite alkene and Sb2S3The hydrothermal synthesis of laminated structure compound
Method, the synthetic method craft is simple, of low cost, and the compound of preparation combines the excellent performance of the two.
The design scheme of the present invention：
It is grown on the Sb of graphene surface2S3Nanometer sheet has sheet Sb for ultra-thin mono-layer graphite surface growth2S3, have
Mesoporous hierarchical organization.
It is grown on the Sb of graphene surface2S3The preparation method of nanometer sheet, includes the following steps：
(1) by magnetic agitation, by SbCl3It is dissolved in ethylene glycol solution, obtains solution A；
(2) it is kept stirring, dodecyl sodium sulfate (SDS) is added to as template in solution A；
(3) Graphene powder of freeze-drying is added in ethylene glycol solution, so that graphene is completely dissolved by ultrasound, obtains
Solution B；
(4) under strong stirring, above-mentioned solution A is mixed with solution B, obtains uniform mixed liquor；
(5) L-cysteine is added into mixed liquor, and stirs 30min, so that it is fully dissolved simultaneously system uniform；
(6) syringe is utilized, above-mentioned system is added dropwise in NaOH solution, needs to keep strong stirring in the process, keep away
It is excessively high to exempt from local basicity；
(7) above-mentioned mixed liquor is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is liner, the constant temperature under 150 DEG C of hydrothermal conditions
Reaction is for 24 hours；
(8) dark brown deposit is obtained after reaction, is washed 3 times with deionized water and absolute ethyl alcohol respectively, the production that will be obtained
Object natural air drying obtains dark-brown product；
(9) in tube furnace, under an ar atmosphere, product burns 3h at 200 DEG C, obtains target product.
Each raw material according to following dosage proportions：
SbCl3Dosage be 0.228g, be dissolved in 15mL ethylene glycol solutions；
The dosage of dodecyl sodium sulfate (SDS) is 0.5g；
The dosage of Graphene powder is 0.003g, is dissolved in 15mL ethylene glycol solutions；
The dosage of L-cysteine is 0.485g；
A concentration of 5mol/L of NaOH solution, dosage 2mL.
It is grown on the Sb of graphene surface2S3The purposes of nanometer sheet, is used to prepare photoelectrocatalysimaterial material.
It is an advantage of the invention that：Synthetic method craft is simple, of low cost, reaction process is mild, obtained product pattern
Well, there is application prospect in photoelectric properties；The Sb of preparation2S3/ graphene composite structure is that ultra-thin mono-layer graphite surface is grown
Sheet Sb2S3, there is mesoporous hierarchical organization, there is higher specific surface area, larger porosity.
Description of the drawings
Fig. 1 is Sb prepared by embodiment2S3The XRD spectrum of/graphene composite structure；
Fig. 2 a are Sb prepared by embodiment2S3One of the SEM spectrum of/graphene composite structure；
Fig. 2 b are Sb prepared by embodiment2S3The two of the SEM spectrum of/graphene composite structure；
Fig. 2 c are Sb prepared by embodiment2S3The three of the SEM spectrum of/graphene composite structure；
Fig. 2 d are Sb prepared by embodiment2S3The four of the SEM spectrum of/graphene composite structure；
Fig. 3 is Sb prepared by embodiment2S3The N2 adsorption of/graphene composite structure-parsing thermoisopleth is bent with pore-size distribution
Line.
Specific implementation mode
It is described in conjunction with the embodiments the specific technical solution of the present invention.
This is grown on the Sb of graphene surface2S3Nanometer sheet, using hydrothermal synthesis method, steps are as follows：
1) by magnetic agitation, by 0.228g SbCl3It is dissolved in 15mL ethylene glycol solutions, obtains solution A；
2) it is kept stirring, 0.5g dodecyl sodium sulfates (SDS) is added to as template in solution A；
3) the 0.003g Graphene powders being freeze-dried are added in 15mL ethylene glycol solutions, ultrasonic 2h keeps graphene complete
Dissolving, obtains solution B；
4) under strong stirring, above-mentioned solution A is mixed with solution B, obtains uniform mixed liquor；
5) 0.485g L-cysteines are added into mixed liquor, and stir 30min, so that it is fully dissolved simultaneously system uniform；
6) syringe is utilized, above-mentioned system is added dropwise in 2mL NaOH (5mol/L) solution, needs to keep in the process
Strong stirring avoids local basicity excessively high；
7) above-mentioned mixed liquor is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is liner, the constant temperature under 150 DEG C of hydrothermal conditions
Reaction is for 24 hours；
8) dark brown deposit is obtained after reaction, is washed 3 times with deionized water and absolute ethyl alcohol respectively, the product that will be obtained
Natural air drying obtains dark-brown product；
9) in tube furnace, under an ar atmosphere, so that sample is burnt 3h at 200 DEG C, obtain target product.
Fig. 1 is Sb prepared by embodiment2S3The XRD spectrum of/graphene composite structure.It can be seen from the figure that sample
Peak and Sb2S3Standard card is corresponding relatively good, and the peak of graphene is blanked substantially.
Fig. 2 a to Fig. 2 d are Sb prepared by embodiment2S3The SEM spectrum of/graphene composite structure.It can be seen that graphene
It is thin, transparent, Sb2S3Thin slice be scattered and be grown on graphene surface.
Fig. 3 is Sb prepared by embodiment2S3The N2 adsorption of/graphene composite structure-parsing thermoisopleth and pore-size distribution are bent
Line.This figure line, which is can be seen that, from N2 adsorption-parsing thermoisopleth belongs to Section IV class absorption-analytic curve, H3 type hysteresis loops.From hole
Diameter distribution curve, the average grain diameter that can obtain this structure are about 22nm, illustrate that the sample of synthesis belongs to typical meso-hole structure.
Claims (4)
1. being grown on the Sb of graphene surface2S3Nanometer sheet, which is characterized in that structure, which is ultra-thin mono-layer graphite surface growth, to be had
Sheet Sb2S3, there is mesoporous hierarchical organization.
2. the Sb according to claim 1 for being grown on graphene surface2S3The preparation method of nanometer sheet, which is characterized in that packet
Include following steps：
(1) by magnetic agitation, by SbCl3It is dissolved in ethylene glycol solution, obtains solution A；
(2) it is kept stirring, is added to dodecyl sodium sulfate as template in solution A；
(3) Graphene powder of freeze-drying is added in ethylene glycol solution, so that graphene is completely dissolved by ultrasound, obtains solution
B；
(4) under strong stirring, above-mentioned solution A is mixed with solution B, obtains uniform mixed liquor；
(5) L-cysteine is added into mixed liquor, and stirs 30min, so that it is fully dissolved simultaneously system uniform；
(6) syringe is utilized, above-mentioned system is added dropwise in NaOH solution, needs to keep strong stirring in the process, avoids office
Portion's basicity is excessively high；
(7) above-mentioned mixed liquor is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is liner, the isothermal reaction under 150 DEG C of hydrothermal conditions
24h；
(8) dark brown deposit is obtained after reaction, is washed 3 times with deionized water and absolute ethyl alcohol respectively, certainly by obtained product
It so air-dries, obtains dark-brown product；
(9) in tube furnace, under an ar atmosphere, so that product is burnt 3h at 200 DEG C, obtain target product.
3. the Sb according to claim 2 for being grown on graphene surface2S3The preparation method of nanometer sheet, which is characterized in that each
Raw material according to following dosage proportions：
SbCl3Dosage be 0.228g, be dissolved in 15mL ethylene glycol solutions；
The dosage of dodecyl sodium sulfate is 0.5g；
The dosage of Graphene powder is 0.003g, is dissolved in 15mL ethylene glycol solutions；
The dosage of L-cysteine is 0.485g；
A concentration of 5mol/L of NaOH solution, dosage 2mL.
4. the Sb according to claim 1 for being grown on graphene surface2S3The purposes of nanometer sheet, which is characterized in that for making
Standby photoelectrocatalysimaterial material.
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| CN201810417304.6A CN108579767A (en) | 2018-05-04 | 2018-05-04 | It is grown on the Sb of graphene surface2S3Nanometer sheet and its preparation method and application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111282591A (en) * | 2020-03-20 | 2020-06-16 | 桂林电子科技大学 | Preparation method of antimony trisulfide/AgI/Ag/BON photocatalyst for soil remediation |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102694171A (en) * | 2012-06-08 | 2012-09-26 | 浙江大学 | Hydrothermal preparation method for composite material of single-layer WS2 and graphene |
| CN105289657A (en) * | 2015-11-30 | 2016-02-03 | 湘潭大学 | Preparation method for graphene and antimony sulphide nano-rod composite visible light catalyst |
| CN106622294A (en) * | 2016-12-31 | 2017-05-10 | 湘潭大学 | Preparation method of graphene-based composite Sb2S3 photocatalyst |
-
2018
- 2018-05-04 CN CN201810417304.6A patent/CN108579767A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102694171A (en) * | 2012-06-08 | 2012-09-26 | 浙江大学 | Hydrothermal preparation method for composite material of single-layer WS2 and graphene |
| CN105289657A (en) * | 2015-11-30 | 2016-02-03 | 湘潭大学 | Preparation method for graphene and antimony sulphide nano-rod composite visible light catalyst |
| CN106622294A (en) * | 2016-12-31 | 2017-05-10 | 湘潭大学 | Preparation method of graphene-based composite Sb2S3 photocatalyst |
Non-Patent Citations (1)
| Title |
|---|
| BAOPING LU等: "Facile, one-pot solvothermal method to synthesize ultrathin Sb2S3 nanosheets anchored on graphene", 《DALTON TRANSACTIONS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111282591A (en) * | 2020-03-20 | 2020-06-16 | 桂林电子科技大学 | Preparation method of antimony trisulfide/AgI/Ag/BON photocatalyst for soil remediation |
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Application publication date: 20180928 |
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