CN105800673A - Method for preparing In4SnS8 ultrathin film - Google Patents
Method for preparing In4SnS8 ultrathin film Download PDFInfo
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- CN105800673A CN105800673A CN201610133452.6A CN201610133452A CN105800673A CN 105800673 A CN105800673 A CN 105800673A CN 201610133452 A CN201610133452 A CN 201610133452A CN 105800673 A CN105800673 A CN 105800673A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/006—Compounds containing, besides tin, two or more other elements, with the exception of oxygen or hydrogen
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a method for preparing an In4SnS8 ultrathin film. The method is characterized by comprising the following steps of: I, preparing precursors, namely, mixing sodium diethyl dithiocarbamate trihydrate with indium salt and tin salt to react respectively, filtering so as to obtain filter cakes, washing the filter cakes, and drying so as to obtain the precursors, that is, indium diethyl dithiocarbamate trihydrate and tin diethyl dithiocarbamate trihydrate; II, performing solvent thermal reaction, namely, dispersing the indium diethyl dithiocarbamate trihydrate and the tin diethyl dithiocarbamate trihydrate in the precursors in a solvent containing a surfactant so as to obtain a mixed liquid, and heating the mixed liquid in a hydrothermal kettle to initiate solvent thermal reaction so as to obtain a product; and III, performing aftertreatment, namely, centrifuging a dispersed liquid containing the product, precipitating, further dissolving in absolute ethyl alcohol, performing ultrasonic dispersion and centrifugal separation, and repeating the ultrasonic dispersion and the centrifugal separation process for multiple times, thereby obtaining the In4SnS8 ultrathin film. The method is simple in process, easy to operate and rapid in preparation speed.
Description
Technical field
The present invention relates to nano semiconductor material field, be specifically related to In4SnS8Ultrathin membrane and preparation method thereof.
Background technology
The semi-conducting material of two-dimensional structure monolayer or few layer, for instance Co3O4, MoS2And CuInS2Nanometer film etc., have big surface-volume than the thickness with atomic scale, thus giving the catalysis of they some uniquenesses, photoelectricity and chemical property, they are expected to for fields such as photoelectric device, sensor, energy conversion and storage devices.The method in the past preparing this type of semiconductor nano film mainly has chemical vapour deposition technique, electro-deposition, spray pyrolysis etc..These methods are typically necessary the preparation condition of harshness, for instance high temperature, fine vacuum, or the shortcoming such as apparatus expensive, complex operation.
In4SnS8Being a kind of multi-element metal sulfide semiconductor material, its band gap is 2.5eV, has visible absorption ability, therefore has potential application in field of solar energy conversion.But at present to In4SnS8Research less, the synthetic method reported mostly is liquid phase synthesizing method, and what obtain mostly is In4SnS8Cluster, it is impossible to obtain the In of two dimension4SnS8Thin film.
Summary of the invention
The present invention proposes for solving the problems referred to above, it is provided that a kind of In4SnS8The preparation method of ultrathin membrane.
A kind of In4SnS8The preparation method of ultrathin membrane, it is characterised in that comprise the following steps:
Step one, prepares presoma:
By diethyl-dithio amidocarbonic acid sodium respectively with indium salts and pink salt hybrid reaction, filter to obtain filter cake, clean filter cake post-drying and prepare presoma and diethyl-dithio amidocarbonic acid indium and diethyl-dithio amidocarbonic acid stannum；
Step 2, solvent thermal reaction:
It is scattered in the solvent containing surfactant by the diethyl-dithio amidocarbonic acid indium in presoma and diethyl-dithio amidocarbonic acid stannum to obtain mixed liquor, heated in water heating kettle by mixed liquor, solvent thermal reaction occurs, obtains product；
Step 3, post processing:
By the dispersion liquid centrifugation containing product, it is precipitated, precipitation is re-dissolved in dehydrated alcohol and carries out ultrasonic disperse and centrifugal separation processes, repeat ultrasonic disperse and namely centrifugal separation processes repeatedly obtains In afterwards4SnS8Ultrathin membrane.
In provided by the invention4SnS8The preparation method of ultrathin membrane, it is also possible to have a feature in that wherein, indium salts includes indium nitrate, indium acetate, indium chloride, and pink salt includes nitric acid stannum, STANNOUS SULPHATE CRYSTALLINE, stannic chloride, stannous chloride.
In provided by the invention4SnS8The preparation method of ultrathin membrane, it is also possible to have a feature in that wherein, the condition of drying is dry 12 hours at 60 DEG C.
In provided by the invention4SnS8The preparation method of ultrathin membrane, it is also possible to have a feature in that wherein, surfactant is the one in alkylamine, alkyl acid, alkylol and alkyl hydrosulfide.
In provided by the invention4SnS8The preparation method of ultrathin membrane, it is also possible to have a feature in that wherein, alkylamine is any one in oleyl amine, lauryl amine, 18-amine., and alkyl acid is oleic acid, and alkyl hydrosulfide is lauryl mercaptan.
In provided by the invention4SnS8The preparation method of ultrathin membrane, it is also possible to have a feature in that wherein, solvent is one or more the mixed solvent in alkane, alkene and alkylol.
In provided by the invention4SnS8The preparation method of ultrathin membrane, it is also possible to have a feature in that wherein, alkane includes hexane, heptane, hexamethylene, and alkene is octadecylene, and alkylol includes methanol, ethanol, ethylene glycol.
In provided by the invention4SnS8The preparation method of ultrathin membrane, it is also possible to have a feature in that wherein, the reaction condition of solvent thermal reaction is: temperature 180-280 DEG C, 5-48 hour response time.
In provided by the invention4SnS8The preparation method of ultrathin membrane, it is also possible to have a feature in that wherein, in step 2, the molar ratio 7:1-1:7 of diethyl-dithio amidocarbonic acid indium and diethyl-dithio amidocarbonic acid stannum in presoma.
Invention effect and effect
In provided by the invention4SnS8The preparation method of ultrathin membrane, adopts one-step synthesis method to prepare, and process is simple, processing ease, and preparation speed is fast.The In of preparation4SnS8For perfect two-dimensional nano membrane structure, it is suitable for field of solar energy conversion.
Accompanying drawing explanation
Fig. 1 is the In prepared by the method according to the invention4SnS8Transmission electron microscope (TEM) photo of ultrathin membrane；
Fig. 2 is the In prepared by the method according to the invention4SnS8High power transmission electron microscope (HRTEM) photo of ultrathin membrane；And
Fig. 3 is the In prepared by the method according to the invention4SnS8X-ray diffraction (XRD) collection of illustrative plates of ultrathin membrane.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reaching purpose and effect and be easy to understand, following example are in conjunction with the accompanying drawing In to the present invention4SnS8The concrete operation step of the preparation method of ultrathin membrane is specifically addressed.
1, presoma is prepared, the aqueous solution of the aqueous solution of indium salts or pink salt with sodium diethyldithiocarbamate (NaDDTC) is mixed respectively, under room temperature, magnetic agitation is after 1 hour, stand 3 hours, filter, and repeatedly clean with deionized water, filter cake respectively obtains diethyl-dithio amidocarbonic acid indium and diethyl-dithio amidocarbonic acid stannum after drying 12 hours at 60 DEG C in baking oven.
2, solvent thermal reaction, metal diethyl-dithio amidocarbonic acid indium and diethyl-dithio amidocarbonic acid stannum are scattered in the solution containing specific surfactant with certain proportion, proceed in water heating kettle after ultrasonic disperse is uniform, heat more than 180 DEG C, and keep 5-48 hour.
3, post processing, after being centrifuged above-mentioned product separating, is re-dissolved in dehydrated alcohol, ultrasonic disperse, centrifugation, and repeats ultrasonic disperse and centrifugation 3 times, it is thus achieved that In4SnS8Ultrathin membrane.
In a preferred embodiment of the invention, in the preparation of presoma, slaine selects indium chloride and stannic chloride to be used for preparing In (DDTC)3With Sn (DDTC)4。
In solvent thermal reaction process, presoma In (DDTC)3With Sn (DDTC)4It is scattered in solvent with the ratio of mol ratio 7:1-1:7, it is preferred to use the ratio of mol ratio 4:1.
Embodiment 1
Fig. 1 is the In prepared by the method for the present embodiment4SnS8Transmission electron microscope (TEM) photo of ultrathin membrane
Fig. 2 is the In prepared by the method for the present embodiment4SnS8High power transmission electron microscope (HRTEM) photo of ultrathin membrane
Fig. 3 is the In prepared by the method for the present embodiment4SnS8X-ray diffraction (XRD) collection of illustrative plates of ultrathin membrane.
(1) In (DDTC) is prepared3Presoma.Weigh 10mmol indium chloride and 30mmol sodium diethyldithiocarbamate (NaDDTC), it is dissolved in 100ml deionized water respectively, sodium diethyldithiocarbamate (NaDDTC) dropwise is added indiumchloride solution, under room temperature, magnetic agitation is after 1 hour, stand 3 hours, repeatedly rinse with deionized water, after sucking filtration, put into baking oven after at 60 DEG C dry 12 hours, to obtain In (DDTC)3Presoma.
(2) Sn (DDTC) is prepared4Presoma.Weigh 10mmol stannic chloride and 40mmol sodium diethyldithiocarbamate (NaDDTC), it is dissolved in 100ml deionized water respectively, sodium diethyldithiocarbamate (NaDDTC) dropwise is added tin chloride solution, under room temperature, magnetic agitation is after 1 hour, stand 3 hours, repeatedly rinse with deionized water, after sucking filtration, put into baking oven after at 60 DEG C dry 12 hours, to obtain Sn (DDTC)4Presoma.
(3) solvent thermal reaction.Weigh 0.1mmolIn (DDTC) respectively3With 0.025mmolSn (DDTC)4, by In (DDTC)3With Sn (DDTC)4It is scattered in the alcoholic solution containing 10mmol oleyl amine.Ultrasonic so as to be completely dispersed.Mixed liquor is proceeded in 50mL water heating kettle, be warming up to 220 DEG C, and keep 24 hours.
(4) post processing.After solution cools down, it is centrifuged product separating, is re-dissolved in dehydrated alcohol, ultrasonic disperse, centrifugation, and repeat ultrasonic disperse and centrifugation 3 times, it is thus achieved that In4SnS8Ultrathin membrane.
To prepared In4SnS8Ultrathin membrane carries out transmission electron microscope (TEM) detection, and testing result is as it is shown in figure 1, the In of gained4SnS8For perfect two-dimensional ultrathin membrane structure.
Further it being done high power transmission electron microscope (HRTEM) test, the thickness of film is approximately 0.89nm as shown in Figure 2.
It being carried out X-ray diffraction (XRD) analyze, the collection of illustrative plates obtained is as it is shown on figure 3, being composed known its by XRD figure is film like.
Embodiment 2
(1) In (DDTC) is prepared3Presoma.Weigh 10mmol indium nitrate and 30mmol sodium diethyldithiocarbamate (NaDDTC), it is dissolved in 100ml deionized water respectively, sodium diethyldithiocarbamate (NaDDTC) dropwise is added indium nitrate solution, under room temperature, magnetic agitation is after 2 hours, stand 1 hour, repeatedly rinse with deionized water, after sucking filtration, put into baking oven after at 60 DEG C dry 12 hours, to obtain In (DDTC)3Presoma.
(2) Sn (DDTC) is prepared4Presoma.Weigh 10mmol STANNOUS SULPHATE CRYSTALLINE and 40mmol sodium diethyldithiocarbamate (NaDDTC), it is dissolved in 100ml deionized water respectively, sodium diethyldithiocarbamate (NaDDTC) dropwise is added STANNOUS SULPHATE CRYSTALLINE solution, under room temperature, magnetic agitation is after 1 hour, stand 3 hours, repeatedly rinse with deionized water, after sucking filtration, put into baking oven after at 60 DEG C dry 12 hours, to obtain Sn (DDTC)4Presoma.
(3) solvent thermal reaction.Weigh 0.175mmolIn (DDTC) respectively3With 0.025mmolSn (DDTC)4, by In (DDTC)3With Sn (DDTC)4It is scattered in the octadecylene solution containing 10mmol oleic acid.Ultrasonic so as to be completely dispersed.Mixed liquor is proceeded in 50mL water heating kettle, be warming up to 180 DEG C, and keep 36 hours.
(4) post processing.After solution cools down, it is centrifuged product separating, is re-dissolved in dehydrated alcohol, ultrasonic disperse, centrifugation, and repeat ultrasonic disperse and centrifugation 3 times, it is thus achieved that In4SnS8Ultrathin membrane.
Embodiment 3
(1) In (DDTC) is prepared3Presoma.Weigh 10mmol indium acetate and 30mmol sodium diethyldithiocarbamate (NaDDTC), it is dissolved in 100ml deionized water respectively, sodium diethyldithiocarbamate (NaDDTC) dropwise is added indium acetate solution, under room temperature, magnetic agitation is after 6 hours, stand 8 hours, repeatedly rinse with deionized water, after sucking filtration, put into baking oven after at 60 DEG C dry 12 hours, to obtain In (DDTC)3Presoma.
(2) Sn (DDTC) is prepared4Presoma.Weigh 10mmol stannous chloride and 40mmol sodium diethyldithiocarbamate (NaDDTC), it is dissolved in 100ml deionized water respectively, sodium diethyldithiocarbamate (NaDDTC) dropwise is added stannous chloride solution, under room temperature, magnetic agitation is after 1 hour, stand 3 hours, repeatedly rinse with deionized water, after sucking filtration, put into baking oven after at 60 DEG C dry 12 hours, to obtain Sn (DDTC)4Presoma.
(3) solvent thermal reaction.Weigh 0.025mmolIn (DDTC) respectively3With 0.175mmolSn (DDTC)4, by In (DDTC)3With Sn (DDTC)4It is scattered in the cyclohexane solution containing 10mmol lauryl mercaptan.Ultrasonic so as to be completely dispersed.Mixed liquor is proceeded in 50mL water heating kettle, be warming up to 280 DEG C, and keep 6 hours.
(4) post processing.After solution cools down, it is centrifuged product separating, is re-dissolved in dehydrated alcohol, ultrasonic disperse, centrifugation, and repeat ultrasonic disperse and centrifugation 3 times, it is thus achieved that In4SnS8Ultrathin membrane.
The effect of embodiment and beneficial effect
The In that above-described embodiment provides4SnS8The preparation method of ultrathin membrane, adopts one-step synthesis method to prepare, and process is simple, processing ease, and preparation speed is fast.Process, TEM, HRTEM, XRD detects confirmation, In prepared by the method4SnS8For perfect two-dimensional nano membrane structure, film thickness, less than 1nm, is suitable for field of solar energy conversion.
Claims (9)
1. an In4SnS8The preparation method of ultrathin membrane, it is characterised in that comprise the following steps:
Step one, prepares presoma:
By diethyl-dithio amidocarbonic acid sodium respectively with indium salts and pink salt hybrid reaction, filter to obtain filter cake, clean described filter cake post-drying and prepare presoma and diethyl-dithio amidocarbonic acid indium and diethyl-dithio amidocarbonic acid stannum；
Step 2, solvent thermal reaction:
It is scattered in the solvent containing surfactant by the diethyl-dithio amidocarbonic acid indium in described presoma and diethyl-dithio amidocarbonic acid stannum to obtain mixed liquor, heated in water heating kettle by described mixed liquor, solvent thermal reaction occurs, obtains product；
Step 3, post processing:
By the described dispersion liquid centrifugation containing product, it is precipitated, described precipitation is re-dissolved in dehydrated alcohol to carry out ultrasonic disperse and centrifugal separation processes, repeat described ultrasonic disperse and namely centrifugal separation processes repeatedly obtains In afterwards4SnS8Ultrathin membrane.
2. according to claim 14SnS8The preparation method of ultrathin membrane, it is characterised in that:
Wherein, described indium salts includes indium nitrate, indium acetate, indium chloride, and described pink salt includes nitric acid stannum, STANNOUS SULPHATE CRYSTALLINE, stannic chloride, stannous chloride.
3. according to claim 14SnS8The preparation method of ultrathin membrane, it is characterised in that:
Wherein, the condition of described drying is dry 12 hours at 60 DEG C.
4. according to claim 14SnS8The preparation method of ultrathin membrane, it is characterised in that:
Wherein, described surfactant is the one in alkylamine, alkyl acid, alkylol and alkyl hydrosulfide.
5. according to claim 44SnS8The preparation method of ultrathin membrane, it is characterised in that:
Wherein, described alkylamine is any one in oleyl amine, lauryl amine, 18-amine.,
Described alkyl acid is oleic acid,
Described alkyl hydrosulfide is lauryl mercaptan.
6. according to claim 14SnS8The preparation method of ultrathin membrane, it is characterised in that:
Wherein, described solvent is one or more the mixed solvent in alkane, alkene and alkylol.
7. according to claim 64SnS8The preparation method of ultrathin membrane, it is characterised in that:
Wherein, described alkane includes hexane, heptane, hexamethylene,
Described alkene is octadecylene,
Described alkylol includes methanol, ethanol, ethylene glycol.
8. according to claim 14SnS8The preparation method of ultrathin membrane, it is characterised in that:
Wherein, the reaction condition of described solvent thermal reaction is: temperature 180-280 DEG C, 5-48 hour response time.
9. according to claim 14SnS8The preparation method of ultrathin membrane, it is characterised in that:
Wherein, in step 2, the molar ratio 7:1-1:7 of diethyl-dithio amidocarbonic acid indium and diethyl-dithio amidocarbonic acid stannum in described presoma.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108821332A (en) * | 2018-07-05 | 2018-11-16 | 苏州影睿光学科技有限公司 | A kind of preparation method of near-infrared stannous sulfide nano particle |
| CN111841577A (en) * | 2020-06-03 | 2020-10-30 | 江苏大学 | Preparation method and application of flaky copper-cobalt bimetallic sulfide catalytic material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101734712A (en) * | 2009-12-30 | 2010-06-16 | 扬州大学 | Method for preparing high-quality copper indium sulfide by employing single-source molecular precursor |
| CN103408065A (en) * | 2013-05-28 | 2013-11-27 | 北京工业大学 | Preparation method of ultrafine nanocrystal Cu2ZnSnS4 |
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2016
- 2016-03-09 CN CN201610133452.6A patent/CN105800673B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101734712A (en) * | 2009-12-30 | 2010-06-16 | 扬州大学 | Method for preparing high-quality copper indium sulfide by employing single-source molecular precursor |
| CN103408065A (en) * | 2013-05-28 | 2013-11-27 | 北京工业大学 | Preparation method of ultrafine nanocrystal Cu2ZnSnS4 |
Non-Patent Citations (2)
| Title |
|---|
| YONGQIAN LEI等: "Cubic spinel In4SnS8: electrical transport properties and electrochemical hydrogen storage properties", 《DALTON TRANSACTIONS》 * |
| YONGQIAN LEI等: "Synthesis, characterization and optical property of flower-like indium tin sulfide nanostructures", 《DALTON TRANSACTIONS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108821332A (en) * | 2018-07-05 | 2018-11-16 | 苏州影睿光学科技有限公司 | A kind of preparation method of near-infrared stannous sulfide nano particle |
| CN111841577A (en) * | 2020-06-03 | 2020-10-30 | 江苏大学 | Preparation method and application of flaky copper-cobalt bimetallic sulfide catalytic material |
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