CN102923761B - Method for synthesizing silver indium sulfide heterojunction structure nano material through hydro-thermal mode - Google Patents
Method for synthesizing silver indium sulfide heterojunction structure nano material through hydro-thermal mode Download PDFInfo
- Publication number
- CN102923761B CN102923761B CN201210439520.3A CN201210439520A CN102923761B CN 102923761 B CN102923761 B CN 102923761B CN 201210439520 A CN201210439520 A CN 201210439520A CN 102923761 B CN102923761 B CN 102923761B
- Authority
- CN
- China
- Prior art keywords
- indium sulfide
- nano
- silver
- indium
- nano material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 17
- YNXRTZDUPOFFKZ-UHFFFAOYSA-N [In].[Ag]=S Chemical compound [In].[Ag]=S YNXRTZDUPOFFKZ-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 23
- 239000000725 suspension Substances 0.000 claims abstract description 16
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 238000010992 reflux Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 239000002243 precursor Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- GKCNVZWZCYIBPR-UHFFFAOYSA-N sulfanylideneindium Chemical compound [In]=S GKCNVZWZCYIBPR-UHFFFAOYSA-N 0.000 claims description 32
- 239000011259 mixed solution Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- 238000013019 agitation Methods 0.000 claims description 16
- 238000006703 hydration reaction Methods 0.000 claims description 12
- 229940055742 indium-111 Drugs 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 11
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 10
- APFVFJFRJDLVQX-AHCXROLUSA-N indium-111 Chemical compound [111In] APFVFJFRJDLVQX-AHCXROLUSA-N 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 230000036571 hydration Effects 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000013543 active substance Substances 0.000 claims description 4
- 238000000703 high-speed centrifugation Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims 1
- AYKOTYRPPUMHMT-UHFFFAOYSA-N silver;hydrate Chemical compound O.[Ag] AYKOTYRPPUMHMT-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 26
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052744 lithium Inorganic materials 0.000 abstract description 14
- 239000008367 deionised water Substances 0.000 abstract description 6
- 239000004094 surface-active agent Substances 0.000 abstract description 4
- 230000002441 reversible effect Effects 0.000 abstract description 2
- 230000001476 alcoholic effect Effects 0.000 abstract 2
- 239000007788 liquid Substances 0.000 abstract 2
- 239000002042 Silver nanowire Substances 0.000 abstract 1
- 239000002131 composite material Substances 0.000 abstract 1
- UKCIUOYPDVLQFW-UHFFFAOYSA-K indium(3+);trichloride;tetrahydrate Chemical compound O.O.O.O.Cl[In](Cl)Cl UKCIUOYPDVLQFW-UHFFFAOYSA-K 0.000 abstract 1
- 210000003739 neck Anatomy 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 9
- 238000011160 research Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 229910052738 indium Inorganic materials 0.000 description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- -1 Indium-111 chlorides Chemical class 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 229910001449 indium ion Inorganic materials 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Landscapes
- Luminescent Compositions (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for synthesizing a silver indium sulfide heterojunction structure nano material through a hydro-thermal mode. The method comprises steps of dissolving an alcoholic suspension of silver nanowires in de-ionized water, stirring the alcoholic suspension, adding indium trichloride tetrahydrate crystal to the mixing liquid, conducting magetic stirring, adding a certain amount of surface active agent cetyl trimethyl ammonium bromide, stirring the surface active agent cetyl trimethyl ammonium bromide till the surface active agent cetyl trimethyl ammonium bromide is dissolved completely, adding a certain amount of thiacetamide, stirring the thiacetamide till the thiacetamide is dissolved completely, regarding the formed mixing liquid as a precursor solution of the silver indium sulfide heterojunction structure nano material, refluxing and heating the precursor solution in a round bottom flask with three necks by using a hydro-thermal method, changing conditions, and obtaining nano structure materials with different shapes. The reaction system is simple, the reaction temperature is low, the synthesized silver indium sulfide structure is novel, the synthesized composite material yield is high, and the reverse specific discharge capacity of the material is high when the material serves as a lithium material cathode. Besides, the method has good repeatability and operability.
Description
Technical field
The present invention relates to preparation method of nano material, especially relate to a kind of method of Hydrothermal Synthesis silver indium sulfide heterogeneous structural nano material.
Background technology
Nano material and nanostructure be the most dynamic in current novel material research field, the future economy and social development are had to the very research object of material impact, be also the most active in nanosecond science and technology, to approach application most important component part.In actual application aspect, because of the semiconductor material such as nano-oxide and sulfide, specific surface area is large, nanostructure is unique, particularly the theoretical specific capacity of lithium cell is large, the advantages such as specific energy density is large, are considered to 21 century be most possibly applied in lithium cell equal energy source memory device as electrode materials.Therefore, the electrochemical research of nano semiconductor material becomes a current very hot research field.In recent years, the oxide compound of various different structures and kind and sulfide nano-material, as nano-electrode materials such as stannic oxide, ferric oxide, moly-sulfide, silicon nanowires and tin, obtain more and more deep research, had very large breakthrough in the performance that discharges and recharges the aspects such as stability, specific storage, high current charge-discharge of lithium cell.But due to nano structural material large volumetric expansion in electrochemical charge and discharge process, the disintegrating of nanostructure, electroconductibility declines, and the existence of initial non-reversible process has seriously hindered the practical application of semiconductor nano material in lithium cell field.Therefore, the exploitation of the electrode materials of new texture is still the interest place of researcher.
Indium trisulfide is very important one in metallic sulfide material, in luminescent material, gas sensitive, solar cell, is studied widely and applies, and it is environmental friendliness thereby the focus that becomes research simultaneously.Existing research is by sonochemistry method, the photochemistry precipitator method, chemical Vapor deposition process at present, hydrothermal method, template etc. have been prepared indium trisulfide nano rod, nanotube and nano-hollow ball etc., specifically can reference: Chem. Mater. 2001,13,2195; J. Mater. Chem. 2002,12,98; Journal of Crystal Growth 2010,312,656; CrystEngComm 2011,13,182 etc.Meanwhile, high (the about 710 mAh g of the lithium cell theoretical capacity of indium sulfide
-1), aspect lithium cell research, indium sulfide also becomes attention (the Cryst. Growth Des. of many seminars, 2009,9,113, J. Mater. Chem., 2011,21,17063, J. Mater. Chem., 2011,21,18398, J. Mater. Chem., 2012,22,11107), but the synthetic of indium sulfide nano material is reaction conditions relative complex mostly, long reaction time, some is the too high security hidden danger of bringing of temperature of reaction, meanwhile, lithium electrical property also remains to be further improved.Therefore the synthetic method of simplicity of design and obtain the more excellent indium sulfide nano structural material of lithium electrical property be still power institute to.
Summary of the invention
A kind of method that the object of this invention is to provide Hydrothermal Synthesis silver indium sulfide heterogeneous structural nano material, adopts hydro-thermal to prepare the hetero nano structure material of the structure uniqueness forming by nano silver wire and around the indium sulfide sheet of nano silver wire growth.
In order to achieve the above object, the step of the technical solution used in the present invention is as follows:
(1) nano silver wire alcohol suspension is added in water solvent, and stirs.
(2) four hydration Indium-111 chloride crystal are joined in (1) step gained mixed solution, be stirred to four hydration Indium-111 chloride solids and fully dissolve.
(3) to the cetyl trimethylammonium bromide powder that adds certain mass in (2) step gained mixed solution, be stirred to powdered and dissolve completely.
(4) in the mixed solution obtaining to (3) step, add a certain amount of thioacetamide, magnetic agitation is to thioacetamide, using gained mixed solution as the precursor of synthesizing silver-colored indium sulfide heterogeneous structure material.
(5) adopt hydrothermal method, by the precursor of (4) step gained reflux in three mouthfuls of round-bottomed flasks, by changing, if do not used nano-silver thread or without conditions such as tensio-active agents, can obtain the nano structural material of different-shape, the product of gained after hydro-thermal is obtained to pistac powder through centrifuge washing, after dry, and this powder is final silver-colored indium sulfide heterogeneous structural nano material.
At the nano silver wire alcohol suspension described in (1) step, the density of this suspension is for being controlled at 0.030g/ml (be in every 1ml nano silver wire alcohol suspension containing the quality control of nano silver wire in 0.030g), and the ratio of nano silver wire alcohol suspension vol used and water solvent volume is 2ml/23ml.
At the add-on 0～0.462g/25ml (not comprising 0 this point) of four hydration Indium-111 chloride crystal described in (2) step.
At the add-on 0～0.520g/25ml of the cetyl trimethylammonium bromide described in (3) step.
At the add-on 0.178g/25ml of the thioacetamide described in (4) step.
Be the wet chemical method heating in a kind of reflux at there-necked flask in the hydrothermal method described in (5) step, Heating temperature is 95 DEG C, and be 80min heat-up time; The pattern of gained silver indium sulfide nanostructure dissimilar materials is the linear structure of nano silver wire and indium sulfide sheet composition; The product obtaining is through high speed centrifugation, and then cleans, obtains pistac powder after dry with analytical pure dehydrated alcohol.
In said process, nano silver wire is bought from Zhejiang Kechuang New Material Technology Co., Ltd., and four hydration Indium-111 chlorides of purity >=97% provide indium ion; Thioacetamide provides sulphur source; Deionization water as solvent; Cetyl trimethylammonium bromide is tensio-active agent.
The beneficial effect that the present invention has is:
1) preparation method is simple, can reach a large amount of preparations, and productive rate exceedes 90%.
2) this is prepared scheme and forms in solution and carry out at water solvent, and raw material is simple, does not introduce any other impurity metal ion, and product purity is high.
3) the silver-colored indium sulfide heterogeneous structural nano material structure novelty preparing, because of the effect of nano-silver thread, the electroconductibility of electrode materials and the stability of structure have had the large material that improves, thereby effectively improve the lithium electrical property of indium sulfide.
Brief description of the drawings
Fig. 1 is the transmission electron microscope photo of the nano silver wire prepared of embodiment 1.
Fig. 2 is the transmission electron microscope photo of the silver-colored indium sulfide heterogeneous structural nano material prepared of embodiment 1.
Fig. 3 is the stereoscan photograph of the silver-colored indium sulfide heterogeneous structural nano material prepared of embodiment 1.
Fig. 4 is the XRD phenogram of the silver-colored indium sulfide heterogeneous structural nano material prepared of embodiment 1.
Fig. 5 is specific surface area and the aperture phenogram of the silver-colored indium sulfide heterogeneous structural nano material prepared of embodiment 1.
Fig. 6 is that the lithium electrical performance data of the silver-colored indium sulfide heterogeneous structural nano material prepared of embodiment 1 characterizes.
Fig. 7 is the stereoscan photograph of the pure indium trisulfide nano structured material prepared of embodiment 2.
Fig. 8 is the stereoscan photograph of the silver-colored indium sulfide hetero nano structure material of the specific morphology prepared of embodiment 3.
Fig. 9 is the synthetic product scanning electron microscope (SEM) photograph of embodiment 4.
Figure 10 is the synthetic product scanning electron microscope (SEM) photograph of example 5.
Embodiment
Embodiment 1:
Carry out according to preparation process.First the alcohol suspension of 2mL nano silver wire is splashed in 23ml deionized water, and magnetic agitation 5 minutes, after 0.231g tetra-hydration Indium-111 chloride solids are added above in mixed solution, magnetic agitation 7 minutes, obtains new mixed solution; Separately add 260mg cetyl trimethylammonium bromide, continue to stir 10 minutes; Finally add 178mg thioacetamide, magnetic agitation 10 minutes, obtains the first body reacting.Mixed solution is injected to three mouthfuls of round-bottomed flasks of 100ml, and be placed in backflow limit, the reaction heated reaction system limit constant temperature of reflux, reaction conditions is: 95 DEG C, and 80min.Solution centrifugal 15min under 10000r/min centrifugation rate after reaction.The solid normal-temperature vacuum repeatedly obtaining after centrifugal 5 times is dried to powder.Transmissioning electric mirror test sample is that the pressed powder obtaining after dry is taken out and is again dispersed on a small quantity in dehydrated alcohol, draws two drop in the clean copper mesh surface that is coated with one deck carbon film with liquid-transfering gun.Sem test sample be by sample drop on silicon chip and stick in aluminium base sample table.Fig. 1 is the transmission electron microscope photo of the nano silver wire bought of embodiment 1, and Fig. 2 has provided the transmission electron microscope photo of the silver-colored indium sulfide heterogeneous structural nano material obtaining according to embodiment 1.Fig. 3 has provided the stereoscan photograph of the silver-colored indium sulfide heterogeneous structural nano material obtaining according to embodiment 1.The pattern of the nano silver wire that used as can be seen from Figure 1, the silver-colored indium sulfide heterogeneous structural nano material of wire is made up of nanometer sheet as can be seen from Figure 2; Can obviously find out that from Fig. 3 silver-colored indium sulfide heterogeneous structural nano material is along the nano silver wire overall pattern forming of growing by indium sulfide sheet.Fig. 4 is that the XRD of the silver-colored indium sulfide heterogeneous structural nano material that obtains according to embodiment 1 characterizes, and as can be seen from the figure matrix material only comprises silver and indium sulfide, and not containing other impurity.Specific surface area and aperture that Fig. 5 has provided the silver-colored indium sulfide heterogeneous structural nano material obtaining according to embodiment 1 characterize, and can show that the specific surface area (BET) of sandwich is up to 31 m from figure
2/ g, aperture mean size is 40 nm.Fig. 6 has provided silver-colored indium sulfide heterogeneous structural nano material that embodiment 1 the obtains lithium electrical property result as negative material, in the time that electrode is worked with the charging and discharging currents of 700 mA/g, its specific storage still has 548 mAh/g after 100 circulations, and the lithium electrical capacity of pure sheet indium sulfide (Fig. 7) is measured as 348 mAh/g in identical conditions, from data, after compound, the lithium electricity specific storage of material has improved nearly 60%.
Embodiment 2:
Carry out according to preparation process.0.231g tetra-hydration Indium-111 chlorides are added in the beaker that fills 25ml deionized water, and magnetic agitation 7 minutes, obtains transparent settled solution; Separately add 260mg cetyl trimethylammonium bromide, continue to stir 10 minutes; Now solution is still clarified, and finally adds 178mg thioacetamide, and magnetic agitation 10 minutes, obtains flaxen solution, and this solution is as the first body of reaction.Solution is injected to three mouthfuls of round-bottomed flasks of 100ml, and as for there being backflow limit, limit constant temperature in the reaction heated reaction system of reflux, reaction conditions is: 95 DEG C, 80min.Solution centrifugal 15min under 10000r/min centrifugation rate after reaction.The solid normal-temperature vacuum repeatedly obtaining after centrifugal 5 times is dried to powder.Sem test sample is that the pressed powder obtaining after dry is taken out and is again dispersed on a small quantity in dehydrated alcohol, draws two drop on clean silicon chip and stick in aluminium base sample table with liquid-transfering gun.Fig. 7 shows that product is sheet indium trisulfide flake nano structure.From scheming, silver-colored line is not participated in when reaction, synthesized sample be the sheet indium sulfide of free accumulation.
Embodiment 3:
Carry out according to preparation process.Carry out according to preparation process.First the alcohol suspension of 2mL nano silver wire is splashed in 23ml deionized water, and magnetic agitation 10 minutes, after 0.231g tetra-hydration Indium-111 chloride solids are added above in mixed solution, magnetic agitation 7 minutes, obtains new mixed solution; Finally add 178mg thioacetamide, magnetic agitation 10 minutes, obtains the first body reacting.Mixed solution is injected to three mouthfuls of round-bottomed flasks of 100ml, and as for there being backflow limit, limit constant temperature in the reaction heated reaction system of reflux, reaction conditions is: 95 DEG C, 80min.Solution centrifugal 15min under 10000r/min centrifugation rate after reaction.The solid normal-temperature vacuum repeatedly obtaining after centrifugal 5 times is dried to powder.Sem test sample is that the pressed powder obtaining after dry is taken out and is again dispersed on a small quantity in dehydrated alcohol, draws two drop on clean silicon chip and stick in aluminium base sample table with liquid-transfering gun.As can be seen from Figure 8, in the time not adding Surfactant CTAB, the sample topography of gained is very inhomogeneous.
Embodiment 4:
Carry out according to preparation process.First, by 2mL, density is that the alcohol suspension of 0.030g/ml nano silver wire splashes in 23ml deionized water, and magnetic agitation 5 minutes, after 0.231g tetra-hydration Indium-111 chloride solids are added above in mixed solution, magnetic agitation 7 minutes, obtains new mixed solution; Separately add 260mg cetyl trimethylammonium bromide, continue to stir 10 minutes; Finally add 178mg thioacetamide, magnetic agitation 10 minutes, obtains the first body reacting.Mixed solution is injected to three mouthfuls of round-bottomed flasks of 100ml, and be placed in backflow limit, the reaction heated reaction system limit constant temperature of reflux, reaction conditions is: 95 DEG C, and 80min.Solution centrifugal 15min under 10000r/min centrifugation rate after reaction.The solid normal-temperature vacuum repeatedly obtaining after centrifugal 5 times is dried to powder.Transmissioning electric mirror test sample is that the pressed powder obtaining after dry is taken out and is again dispersed on a small quantity in dehydrated alcohol, draws two drop in the clean copper mesh surface that is coated with one deck carbon film with liquid-transfering gun.Sem test sample be by sample drop on silicon chip and stick in aluminium base sample table.Fig. 9 shows the product scanning electron microscope (SEM) photograph that this example is synthetic.From scheming, when the amount of silver-colored line doubles, the sheet indium sulfide that is still silver-colored line and free accumulation of synthesized sample.But because silver-colored line amount doubles, the indium sulfide sheet of piling up on silver-colored line seems loose.
Embodiment 5:
Carry out according to preparation process.First the alcohol suspension of 2mL nano silver wire is splashed in 23ml deionized water, and magnetic agitation 5 minutes, after 0.231g tetra-hydration Indium-111 chloride solids are added above in mixed solution, magnetic agitation 7 minutes, obtains new mixed solution; Separately add 520mg cetyl trimethylammonium bromide, continue to stir 10 minutes; Finally add 178mg thioacetamide, magnetic agitation 10 minutes, obtains the first body reacting.Mixed solution is injected to three mouthfuls of round-bottomed flasks of 100ml, and be placed in backflow limit, the reaction heated reaction system limit constant temperature of reflux, reaction conditions is: 95 DEG C, and 80min.Solution centrifugal 15min under 10000r/min centrifugation rate after reaction.The solid normal-temperature vacuum repeatedly obtaining after centrifugal 5 times is dried to powder.Transmissioning electric mirror test sample is that the pressed powder obtaining after dry is taken out and is again dispersed on a small quantity in dehydrated alcohol, draws two drop in the clean copper mesh surface that is coated with one deck carbon film with liquid-transfering gun.Sem test sample be by sample drop on silicon chip and stick in aluminium base sample table.Figure 10 shows the product scanning electron microscope (SEM) photograph synthetic according to example 5.From scheming, when tensio-active agent doubles, the indium sulfide pattern of silver-colored line surface attachment is substantially constant.
Claims (1)
1. a method for Hydrothermal Synthesis silver indium sulfide heterogeneous structural nano material, is characterized in that the step of the method is as follows:
(1) nano silver wire alcohol suspension is added in water solvent, and stirs;
(2) four hydration Indium-111 chloride crystal are joined in (1) step gained mixed solution, be stirred to four hydration Indium-111 chloride solids and fully dissolve;
(3) to the cetyl trimethylammonium bromide powder that adds certain mass in (2) step gained mixed solution, be stirred to powdered and dissolve completely;
(4) in the mixed solution obtaining to (3) step, add a certain amount of thioacetamide, magnetic agitation is to thioacetyl amine solvent, using gained mixed solution as the precursor of synthesizing silver-colored indium sulfide heterogeneous structure material;
(5) adopt hydrothermal method, by the precursor of (4) step gained reflux in three mouthfuls of round-bottomed flasks, by change condition, can obtain the nano material of different-shape, the product of gained after hydro-thermal is obtained to pistac powder through centrifuge washing, after dry, this powder is final silver-colored indium sulfide heterogeneous structural nano material, and described condition is: plus nano silver line;
At the nano silver wire alcohol suspension described in (1) step, the density of this suspension is for being controlled at 0.030g/mL, be in every 1mL nano silver wire alcohol suspension containing the quality of nano silver wire at 0.030g, the ratio of the suspension vol of described nano silver wire and water solvent volume is 2mL/23mL;
Add-on at four hydration Indium-111 chloride crystal described in (2) step is controlled at 0.231g/25mL;
Add-on at the tensio-active agent cetyl trimethylammonium bromide described in (3) step is 0～0.520g/25mL;
Add-on at the thioacetamide described in (4) step is 0.178g/25mL;
Be the wet chemical method heating in a kind of reflux at there-necked flask in the hydrothermal method described in (5) step, Heating temperature is 95 DEG C, and be 80min heat-up time; The pattern of gained silver indium sulfide nanostructure dissimilar materials is the linear structure of nano silver wire and indium sulfide sheet composition; The product obtaining is through high speed centrifugation, and then cleans, obtains pistac powder after dry with analytical pure dehydrated alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210439520.3A CN102923761B (en) | 2012-11-06 | 2012-11-06 | Method for synthesizing silver indium sulfide heterojunction structure nano material through hydro-thermal mode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210439520.3A CN102923761B (en) | 2012-11-06 | 2012-11-06 | Method for synthesizing silver indium sulfide heterojunction structure nano material through hydro-thermal mode |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102923761A CN102923761A (en) | 2013-02-13 |
| CN102923761B true CN102923761B (en) | 2014-07-23 |
Family
ID=47638725
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210439520.3A Expired - Fee Related CN102923761B (en) | 2012-11-06 | 2012-11-06 | Method for synthesizing silver indium sulfide heterojunction structure nano material through hydro-thermal mode |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102923761B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104843769B (en) * | 2015-04-09 | 2016-08-17 | 首都师范大学 | By the controlled method preparing indium sulfide ultra-thin two-dimension nano material of metal ion and the purposes of this material |
| CN116351438B (en) * | 2023-04-28 | 2024-09-10 | 齐鲁工业大学(山东省科学院) | Cerium oxide indium sulfide photocatalytic material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054200A (en) * | 2007-05-17 | 2007-10-17 | 上海交通大学 | Method of preparing monodisperse ternary sulfide CuInS2 |
| CN102303900A (en) * | 2011-08-18 | 2012-01-04 | 浙江大学 | Hydrothermal synthesizing method of sheet-formed diindium trisulphide nano-structured material |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101462653B1 (en) * | 2008-05-20 | 2014-11-17 | 삼성전자 주식회사 | Preparing Method of Nano particle using Carbene derivative |
| US20120066956A1 (en) * | 2009-05-29 | 2012-03-22 | Abobelo Da | Terminal fly fishing tackle |
-
2012
- 2012-11-06 CN CN201210439520.3A patent/CN102923761B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054200A (en) * | 2007-05-17 | 2007-10-17 | 上海交通大学 | Method of preparing monodisperse ternary sulfide CuInS2 |
| CN102303900A (en) * | 2011-08-18 | 2012-01-04 | 浙江大学 | Hydrothermal synthesizing method of sheet-formed diindium trisulphide nano-structured material |
Non-Patent Citations (8)
| Title |
|---|
| 《Fabrication of indium sulfide nanofibers via a hydrothermal method assisted by AAO template》;Xiaoyi Zhu et al.;《Materials Research Bulletin》;20060310;第41卷;第1584–1588页 * |
| 《Single-source precursors to ternary silver indium sulfide materials》;Theivanayagam C. Deivaraj et al.;《Chem. Commun.》;20011024;第2304–2305页 * |
| 《The physical properties and photoresponse of AgIn5S8 polycrystalline》;Kong-Wei Cheng et al.;《Journal of Photochemistry and Photobiology A: Chemistry》;20070323;第190卷;第77-87页 * |
| Fangmin Ye et al..《A heterostructured Ag@In2S3 composite with enhanced lithium storage capacity》.《Journal of Materials Chemistry A》.2013,第1卷第5208–5211页. |
| Fangmin Ye et al..《A heterostructured AgIn2S3 composite with enhanced lithium storage capacity》.《Journal of Materials Chemistry A》.2013,第1卷第5208–5211页. * |
| Kong-Wei Cheng et al..《The physical properties and photoresponse of AgIn5S8 polycrystalline》.《Journal of Photochemistry and Photobiology A: Chemistry》.2007,第190卷第77-87页. |
| Theivanayagam C. Deivaraj et al..《Single-source precursors to ternary silver indium sulfide materials》.《Chem. Commun.》.2001,第2304–2305页. |
| Xiaoyi Zhu et al..《Fabrication of indium sulfide nanofibers via a hydrothermal method assisted by AAO template》.《Materials Research Bulletin》.2006,第41卷第1584–1588页. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102923761A (en) | 2013-02-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Lu et al. | Synthesis of nickel chalcogenide hollow spheres using an l-cysteine-assisted hydrothermal process for efficient supercapacitor electrodes | |
| CN109553779B (en) | Preparation method and application of three-dimensional nanoflower metal organic framework material | |
| CN108417404B (en) | A kind of preparation method of electrode material for super capacitor | |
| CN104134783B (en) | Nano nickel sulphide/grapheme composite positive electrode material and preparation method thereof | |
| CN103326007B (en) | The preparation method of three-dimensional graphite thiazolinyl tin dioxide composite material and application thereof | |
| CN106450205A (en) | Two-dimensional transition metal carbide (nitride) and nano sulfur particle composite material and preparation and application thereof | |
| CN105742602A (en) | Sn/MoS<2>/C composite material for sodium ion battery negative electrode and preparation method therefor | |
| CN107452951B (en) | XS2@YSe2The preparation method of the anode material of lithium-ion battery of core-shell structure | |
| CN108855145B (en) | Two-step method for preparing cobalt sulfide/molybdenum sulfide composite material and application of cobalt sulfide/molybdenum sulfide composite material in hydrogen evolution reaction | |
| CN105883940B (en) | Preparation method of block NiS2 and application of block NiS2 to sodium-ion battery | |
| Chen et al. | MOF-derived Mo-CoP@ NiFe LDH hierarchical nanosheets for high-performance hybrid supercapacitors | |
| CN102910615A (en) | Preparation method of graphene oxide/iron disulfide composite nano particles | |
| Ahmad et al. | Graphene oxide selenium nanorod composite as a stable electrode material for energy storage devices | |
| CN106952737A (en) | A kind of preparation method of tungsten disulfide flake nano material | |
| CN111921529A (en) | Preparation method and application of nickel-cobalt metal organic framework/nickel-cobalt metal hydroxide heterogeneous material | |
| CN106847530A (en) | A kind of nickel cobalt base-carbon nano tube combination electrode material and preparation method thereof | |
| CN104658771B (en) | A kind of preparation method and application of sea urchin shape vanadium base nano-electrode material | |
| Khan et al. | Engineering N-reduced graphene oxide wrapped Co3O4@ f-MWCNT hybrid for enhance performance dye-sensitized solar cells | |
| Liu et al. | Microwave synthesis of NiSe/NiTe2 nanocomposite grown in situ on Ni foam for all-solid-state asymmetric supercapacitors | |
| Chen et al. | Interface regulation strategy in constructing ZnS@ MoS2 heterostructure with enhanced surface reaction dynamics for robust lithium-ion storage | |
| Liu et al. | A novel propeller-like Si@ WO3@ C with boosted electrochemical properties as anode material for lithium-ion batteries | |
| CN109065874A (en) | A kind of MoO3/ rGO-N nanocomposite and its preparation method and application | |
| Zhang et al. | Urchin-like alkaline nickel–cobalt carbonate derived Ni3S4/Co3S4 nanoparticles anchored on rGO for lithium/sodium-ion batteries with enhanced capacity | |
| CN102923761B (en) | Method for synthesizing silver indium sulfide heterojunction structure nano material through hydro-thermal mode | |
| CN105206816A (en) | Preparation method of nickel sulfide-graphene nano composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140723 |