CN105819512A - Quick preparation method of transitional metal sulfide - Google Patents
Quick preparation method of transitional metal sulfide Download PDFInfo
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- CN105819512A CN105819512A CN201610210662.0A CN201610210662A CN105819512A CN 105819512 A CN105819512 A CN 105819512A CN 201610210662 A CN201610210662 A CN 201610210662A CN 105819512 A CN105819512 A CN 105819512A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a preparation method of transitional metal sulfide. By the use of a Na2S/S aqueous solution, the preparation method mainly comprises oxidation and reduction (or hydrothermal method), PMMA spinning and FeCl3/HCl etching. The process is quick, simple and convenient; a large area of flexible thin film sample can be prevented and shows excellent properties such as electro-catalysis, photo-catalysis and solar battery. The transitional metal sulfide prepared by the method has a significant application prospect in the fields of electro-catalysis, energy storage devices (such as a lithium ion battery, a lithium-sulfur battery and a sodium ion battery), photo-catalysis, sensors and the like.
Description
Technical field
The invention belongs to technical field of nano material, relate to the fast preparation method of a kind of transient metal sulfide.
Background technology
Transient metal sulfide (TMDs) has 3d valency electron shell structurre, has visible-range band gap, has the two-dimensional layered structure similar with Graphene, result in they anisotropy on electricity, chemistry, mechanics and thermal property.Based on this, transient metal sulfide obtains a wide range of applications at aspects such as solaode, sensor, lithium ion batteries, and has splendid performance.The transient metal sulfide of 4-7 race is mainly stratiform, and the transient metal sulfide of 8-10 race is unstratified.As one typical two-dimensional layer transient metal sulfide, molybdenum bisuphide (MoS2) because its abundant physics and chemical property cause greatly concern in the recent period, it all obtains application, and excellent performance in fields such as sensor, catalysis, lithium ion batteries.Compared with traditional block materials, nanoscale MoS2、WS2There is more excellent optical, electrical performance.Cobalt sulfide also receives greatly concern because of character and the potential application of its excellence, as in industrial circle, it is widely used in hydrodesulfurization as catalyst, excellent additionally, due to its electrocatalysis characteristic, is also received significant attention as electrochemical capacitor and cathode material for lithium ion battery.Nickel sulfide (NiS) is the semi-conducting material that a class is important, when temperature exceedes its critical temperature, NiS can produce magnetic and electric conductivity conversion of energy, is changed into anti-ferromagnetic quasiconductor, all has at the aspect such as battery material, hydrogenation catalyst at present and study widely.Meanwhile, due to the important application prospect at aspects such as electro-catalysis, photocatalysis, lithium ion batteries, other transient metal sulfide is (such as FeS2、Cu2S, ZnS etc.) also cause the concern of people.Such as, cuprous sulfide (Cu2S) it is the p-type semiconductor material of a kind of low energy gap (Eg=1.2eV), at high temperature there is stronger ionic conductivity, have good luminescence generated by light, main ultrared passes through simultaneously, the performances such as optical characteristics and visible absorption such as catalysis activity, response speed, have a wide range of applications in fields such as photocatalysis, solaode, lithium ion (sodium ion) batteries.
Preparation method about transient metal sulfide mainly has hydro-thermal method, chemical vapour deposition technique, high temperature solid-state method, template etc. at present, and preparation method is the most more complicated.
Summary of the invention
For the shortcoming overcoming above-mentioned prior art, it is an object of the invention to provide the fast preparation method of a kind of transient metal sulfide, combine redox reaction and class Graphene lithographic technique, technical process is simple, quick and convenient, and products therefrom shows more excellent electro-catalysis, photocatalysis performance, in electro-catalysis, photocatalysis, field such as lithium ion (sodium ion) battery, sensor etc., there is good application prospect, the cuprous sulfide (Cu that typical product such as thickness is controlled2S) thin film etc..
To achieve these goals, the technical solution used in the present invention is:
The fast preparation method of a kind of transient metal sulfide, comprises the steps:
(1) by Na2S with S mixes and adds in deionized water, and heating in water bath obtains Na2S/S solution；
(2) by metal in gained Na2S/S solution soaks a period of time, takes out afterwards and clean and be dried, form layer of metal sulfide film in metal surface；
(3) by spin coating PMMA solution on metal sulfide thin film that the substrate of gained is metal, it is dried afterwards；
(4) by the sample that is dried to obtain at FeCl3/ HCl solution performs etching and obtains metal sulfide film sample；
(5) gained metal sulfide film sample is transferred on required base material and is dried；
(6) PMMA is removed.
In described step (1), Na2The mass ratio of S Yu S is 1:20, Na2S/S concentration in deionized water is 0.01-50mol/L, and condition of water bath heating is 30-90 DEG C, 10-60min.
In described step (2), metal is Cu, Fe, Ni or Zn, when for Fe or Ni, heats in immersion process, and heating condition is 80-300 DEG C (preferably 100-200 DEG C), 1-90h (preferably 1-50h)；When for Cu or Zn, soak time is 1s to 1 day.
In described step (2), metal is foam copper or Copper Foil that thickness is 5 μm-100cm, or is iron plate, foamed iron, iron wire or iron powder, or is nickel sheet or nickel foam.
In described step (2), metal is adding Na2Before S/S solution, first soak with diluted acid, to remove the oxide layer on surface, or, in described step (2), metal-oxide is soaked in diluted acid and obtains metal, then metal is added Na2S/S solution.
Described diluted acid is dilute hydrochloric acid, dilute sulfuric acid or spirit of vinegar, and soak time is 1-1000s.
FeCl in described step (4)3/ HCl solution concentration is 0.1-10mol/L.
The base material used in described step (5) is silicon chip, glass carbon plate, polyethylene terephthalate (PET) or polyimides (PI).
The method removing PMMA in described step (6) is repeatedly to soak in acetone, aqueous isopropanol.
Compared with prior art, preparation technology of the present invention mainly includes oxidoreduction (or hydro-thermal method), PMMA spin coating and FeCl3/ HCl etching process, its technique is fast and convenient, can prepare large area flexible film sample, the most also shows the electro-catalysis of excellence, photocatalysis, photodetection performance.The transient metal sulfide utilizing this method to prepare will have good application prospect in fields such as clean energy resource (such as hydrogen), energy storage device (such as lithium ion battery, lithium-sulfur cell, sodium-ion battery), photocatalytic degradation, photodetections.
Accompanying drawing explanation
Fig. 1 is embodiment of the present invention gained Cu2Scanning electron microscope (SEM) photo of S sample, wherein a is embodiment 1 gained Cu2S sample, b is embodiment 3 gained Cu2S sample.
Fig. 2 is the embodiment of the present invention 2 gained Cu2The typical pattern of S sample, wherein a is scanning electron microscope (SEM) photo, b transmission electron microscope (TEM) photo.
Fig. 3 is the embodiment of the present invention 2 gained Cu2Surface profile (surfaceprofile) figure of S sample.
Fig. 4 is the embodiment of the present invention 3 gained Cu2Surface profile (surfaceprofile) figure of S sample.
Fig. 5 is scanning electron microscope (SEM) photo of sample in the embodiment of the present invention, Cu during wherein a is embodiment 52O sample, b is Cu in embodiment 42S sample.
Fig. 6 is scanning electron microscope (SEM) photo of sample in the embodiment of the present invention, NiS sample during wherein a is embodiment 6, and b is FeS in embodiment 72Sample.
Fig. 7 is the embodiment of the present invention 3 gained Cu2The electrocatalytic hydrogen evolution performance schematic diagram of S sample, wherein a is linear VA characteristic curve；B is the Tafel slope that in a, various materials are corresponding.
Fig. 8 is the embodiment of the present invention 4 gained Cu2The Photocatalytic Degradation Property schematic diagram of S sample.
Detailed description of the invention
The present invention provides a kind of chemical attack or solvent thermal technique to the method preparing transient metal sulfide.Below in conjunction with the accompanying drawings and the specific embodiments the present invention is further described.
Embodiment 1
Na2The preparation of S/S solution: by 1.6gS and 12gNa2S adds in 50mL deionized water, is placed in 60 DEG C of stirring in water bath 30min, forms 1MNa2S/S solution.
Cu2The preparation of S: the Copper Foil that 0.127mm is thick is cut to a certain size (1*2cm2), it is placed in 1MNa2S/S solution soaks 2s, takes out and be washed with deionized water clean and be dried.
Cu2The transfer of S: Cu2S surface spin coating PMMA, is placed on 0.5mol/LFeCl3In/HCl solution, being used for etching substrate Cu, soaking and washing is clean the most repeatedly, is finally transferred in required substrate and is dried.Use to soak in acetone and isopropanol and remove PMMA.
Can be used for electro-catalysis, photocatalysis, photodetection, lithium ion/sodium-ion battery performance test afterwards.
Embodiment 2
Consistent with embodiment 1, differ only at preparation Na2During S/S solution, take 1MNa in 5mL embodiment 12S/S solution, then take 45mL deionized water mix homogeneously, form 0.1MNa2S/S solution.
Embodiment 3
Consistent with embodiment 2, differ only in Cu2Copper sheet is placed in 1MNa by S preparation process2S/S solution soaks 15s.
Embodiment 4
Consistent with embodiment 1, differ only at preparation Na2During S/S solution, deionized water volume changes 25mL into.
Embodiment 5
Cu2The preparation of O: a certain size Copper Foil being placed in tube furnace and burns 72h in 500 DEG C of skies, copper sheet surface is oxidized to form Cu2O layer.
Na2The preparation of S/S solution is consistent with embodiment 1.
Cu2The preparation of S: by a certain size (1*2cm2) Cu2O (is attached to copper sheet surface), is placed in 1MNa2S/S solution soaks 5min, takes out and be washed with deionized water clean and be dried.
Embodiment 6
Na2The preparation of S/S solution is consistent with embodiment 1.
Nickel foam is placed in equipped with Na2In the reactor of S/S solution, react 5h in 180 DEG C.Reaction is taken out sample deionized water after terminating and is rinsed well and be dried.
Embodiment 7
Na2The preparation of S/S solution is consistent with embodiment 1.
Iron plate is placed in equipped with Na2In the reactor of S/S solution, react 5h in 180 DEG C.Reaction is taken out sample deionized water after terminating and is rinsed well and be dried.
Embodiment 8
Na2The preparation of S/S solution is consistent with embodiment 1.
Zinc powder is placed in the Na of preparation2S/S solution soaks 30s, takes out ionized water of taking away afterwards and clean and be dried.
The Cu prepared2S uses the extracting mode being similar to Graphene, first at Cu2S surface spin coating PMMA, afterwards at FeCl3Solution etches, cleans up and obtain flexible Cu2S thin film.Afterwards by this flexibility Cu2S thin film is attached to glassy carbon electrode surface, is soaked in the most respectively in acetone, isopropanol to remove PMMA, is dried afterwards and i.e. can be used for electrocatalysis characteristic sign.Experiment uses three-electrode system, uses graphite electrode electrode as a comparison, and saturated calomel electrode is as reference electrode, 0.5mol/LH2SO4Solution is as electrolyte.Utilizing electrochemical workstation, use linear voltammetric scan, sweep speed is set to 10mV/s, and sweep interval is set to 0V to-1V.
NiS and FeS prepared2Sample is directly available in electrocatalysis characteristic test.Experiment silver electrode folder clamps the sample of certain area, as working electrode.It addition, use platinum electrode electrode as a comparison, saturated calomel electrode is as reference electrode, and 1mol/LKOH solution is as electrolyte.Utilizing electrochemical workstation, use linear voltammetric scan, sweep speed is set to 10mV/s, and sweep interval is set to 0V to-1V.
The Cu prepared2S can be used for photocatalytic degradation of dye.Owing to the band gap of this material is only 1.2eV, very strong to visible absorption, make full use of full spectrum segment, 40ummolMB is placed in beaker, puts into sample, be placed under xenon lamp irradiation, sampling in every ten minutes is once.
Fig. 1 a is the Cu using embodiment 1 to prepare2The scanning electron microscope (SEM) photograph of S sample, the most in the form of sheets structure, lamella is bigger and thick, but sheet interlayer has more space.
Fig. 2 a, b are respectively the Cu using embodiment 2 to prepare2The scanning electron microscope (SEM) photograph of S sample and transmission electron microscope picture, this sample has more multi-layer sheet structure, and compares Fig. 1 a, and this lamellar structure size is less.
Fig. 1 b is the Cu using embodiment 3 to prepare2The scanning electron microscope (SEM) photograph of S sample, it is thicker that the lamellar structure of this sample compares Fig. 2, but division occurs in lamella.
Fig. 3 is the Cu using embodiment 2 to prepare2The surface profile map of S sample, from test result it can be seen that use the Cu that embodiment 2 prepares2The average thickness of S thin film is about 20nm.
Fig. 4 is the Cu using embodiment 3 to prepare2The surface profile map of S sample, from test result it can be seen that use the Cu that embodiment 3 prepares2The average thickness of S thin film is about 138nm.
Fig. 5 a is Cu in embodiment 52The scanning electron microscope (SEM) photograph of O nano wire, surface is smoother, and b is Cu2The Cu that O obtains after vulcanizing treatment2The scanning electron microscope (SEM) photograph of S sample, front and back contrasts it can be seen that nanowire surface generates more particulate matter after vulcanizing treatment.
Fig. 6 a is the scanning electron microscope (SEM) photograph of the NiS sample that embodiment 6 prepares, it can be seen that this sample has more gap structure.Fig. 6 b is the FeS that embodiment 7 prepares2The scanning electron microscope (SEM) photograph of sample, in the cubic structure of rule.
Fig. 7 is the Cu that embodiment 3 prepares2Acid medium (the 0.5MH that S sample is corresponding2SO4) electrocatalysis characteristic.A figure is linear VA characteristic curve, and b figure illustrates the Tafel slope figure of its correspondence, and in acid medium, the unlatching current potential of this sample is about-0.4V as we can see from the figure, and Tafel slope is 30mV/dec.
Fig. 8 is the Cu using embodiment 3 to prepare2The schematic diagram of the photocatalytic degradation methylene blue that S sample is corresponding, utilizes visible ray photometer to test its absorption to light, and as seen from the figure, peak value is reducing, and Cu is described2S serves good photodegradation.
Claims (9)
1. the fast preparation method of a transient metal sulfide, it is characterised in that comprise the steps:
(1) by Na2S with S mixes and adds in deionized water, and heating in water bath obtains Na2S/S solution；
(2) by metal in gained Na2S/S solution soaks a period of time, takes out afterwards and clean and be dried, form layer of metal sulfide film in metal surface；
(3) by spin coating polymethyl methacrylate (PMMA) solution on metal sulfide thin film that the substrate of gained is metal, it is dried afterwards；
(4) by the sample that is dried to obtain at FeCl3/ HCl solution performs etching and obtains metal sulfide film sample；
(5) gained metal sulfide film sample is transferred on required base material and is dried；
(6) PMMA is removed.
The fast preparation method of transient metal sulfide the most according to claim 1, it is characterised in that in described step (1), Na2The mass ratio of S Yu S is 1:20, Na2S/S concentration in deionized water is 0.01-50mol/L, and condition of water bath heating is 30-90 DEG C, 10-60min.
The most according to claim 1, the fast preparation method of transient metal sulfide, it is characterised in that in described step (2), metal is Cu, Fe, Ni or Zn, when for Fe or Ni, heats in immersion process, and heating condition is 80-300 DEG C, 1-90h；When for Cu or Zn, soak time is 1s to 1 day.
The fast preparation method of transient metal sulfide the most according to claim 1, it is characterized in that, in described step (2), metal is foam copper or Copper Foil that thickness is 5 μm-100cm, or be iron plate, foamed iron, iron wire or iron powder, or it is nickel sheet or nickel foam.
The most according to claim 1, the fast preparation method of transient metal sulfide, it is characterised in that in described step (2), metal is adding Na2Before S/S solution, first soak with diluted acid, to remove the oxide layer on surface, or, in described step (2), metal-oxide is soaked in diluted acid and obtains metal, then metal is added Na2S/S solution.
The most according to claim 1, the fast preparation method of transient metal sulfide, it is characterised in that described diluted acid is dilute hydrochloric acid, dilute sulfuric acid or spirit of vinegar, soak time is 1-1000s.
The fast preparation method of transient metal sulfide the most according to claim 1, it is characterised in that FeCl in described step (4)3/ HCl solution concentration is 0.1-10mol/L.
The fast preparation method of transient metal sulfide the most according to claim 1, it is characterized in that, the base material used in described step (5) is silicon chip, glass carbon plate, polyethylene terephthalate (PET) or polyimides (PI).
The fast preparation method of transient metal sulfide the most according to claim 1, it is characterised in that the method removing PMMA in described step (6) is repeatedly to soak in acetone, aqueous isopropanol.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106757367A (en) * | 2017-01-04 | 2017-05-31 | 安阳师范学院 | The preparation method of high length-diameter ratio nickel sulfide monocrystal nano line array |
| CN107090586A (en) * | 2017-04-13 | 2017-08-25 | 上海应用技术大学 | A kind of FeS2RGO composites, preparation method and applications |
| CN109671571A (en) * | 2018-06-08 | 2019-04-23 | 天津大学 | A kind of preparation method of fabricated in situ multicomponent metal sulfide composite material |
| CN110699660A (en) * | 2019-10-09 | 2020-01-17 | 昆明理工大学 | Method for rapidly growing cuprous sulfide nanosheet array film on any substrate |
| CN111185198A (en) * | 2020-01-20 | 2020-05-22 | 曲阜师范大学 | Ni/NiO/Ni3S2Catalyst, preparation method and application thereof |
| CN111354931A (en) * | 2020-03-09 | 2020-06-30 | 天津师范大学 | Lithium-sulfur battery positive electrode composite material with high active substance content and preparation method and application thereof |
| CN112103092A (en) * | 2020-07-27 | 2020-12-18 | 浙江工业大学 | Metal cation doped cobalt polysulfide/cobalt hydroxide composite material and preparation method and application thereof |
| CN114560502A (en) * | 2020-11-27 | 2022-05-31 | 国电南瑞科技股份有限公司 | Three-dimensional nano molybdenum-based lithium ion battery cathode material and preparation method thereof |
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| CN106757367A (en) * | 2017-01-04 | 2017-05-31 | 安阳师范学院 | The preparation method of high length-diameter ratio nickel sulfide monocrystal nano line array |
| CN106757367B (en) * | 2017-01-04 | 2018-12-04 | 安阳师范学院 | The preparation method of high length-diameter ratio nickel sulfide monocrystal nano line array |
| CN107090586A (en) * | 2017-04-13 | 2017-08-25 | 上海应用技术大学 | A kind of FeS2RGO composites, preparation method and applications |
| CN109671571A (en) * | 2018-06-08 | 2019-04-23 | 天津大学 | A kind of preparation method of fabricated in situ multicomponent metal sulfide composite material |
| CN110699660A (en) * | 2019-10-09 | 2020-01-17 | 昆明理工大学 | Method for rapidly growing cuprous sulfide nanosheet array film on any substrate |
| CN111185198A (en) * | 2020-01-20 | 2020-05-22 | 曲阜师范大学 | Ni/NiO/Ni3S2Catalyst, preparation method and application thereof |
| CN111354931A (en) * | 2020-03-09 | 2020-06-30 | 天津师范大学 | Lithium-sulfur battery positive electrode composite material with high active substance content and preparation method and application thereof |
| CN112103092A (en) * | 2020-07-27 | 2020-12-18 | 浙江工业大学 | Metal cation doped cobalt polysulfide/cobalt hydroxide composite material and preparation method and application thereof |
| CN114560502A (en) * | 2020-11-27 | 2022-05-31 | 国电南瑞科技股份有限公司 | Three-dimensional nano molybdenum-based lithium ion battery cathode material and preparation method thereof |
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Application publication date: 20160803 |