CN106277064A - A kind of method preparing rhenium disulfide nanometer sheet - Google Patents
A kind of method preparing rhenium disulfide nanometer sheet Download PDFInfo
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- CN106277064A CN106277064A CN201610580163.0A CN201610580163A CN106277064A CN 106277064 A CN106277064 A CN 106277064A CN 201610580163 A CN201610580163 A CN 201610580163A CN 106277064 A CN106277064 A CN 106277064A
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- nanometer sheet
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G47/00—Compounds of rhenium
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses a kind of method preparing rhenium disulfide nanometer sheet, belong to New Two Dimensional field of nano material preparation.The present invention using ammonium perrhenate as rhenium source, thiourea as sulfur source, above-mentioned three kinds of reactants, as reducing agent, are dissolved in aqueous solvent by oxammonium hydrochloride., chemical reaction is there is by regulation reaction temperature and response time, then by product cleaning, after drying processes, final synthesis rhenium disulfide nanometer sheet.Operating process of the present invention is simple, and efficiency is high, reproducible, low cost, can be prepared on a large scale out high-quality rhenium disulfide nanometer sheet, and meanwhile, the present invention is that rhenium disulfide nanometer sheet provides reliable sample preparation methods in the application of electrical and optical aspect.
Description
Technical field
The invention belongs to New Two Dimensional field of nano material preparation, a kind of side preparing rhenium disulfide nanometer sheet
Method.
Background technology
Two-dimensional semiconductor is a kind of emerging electronic material with Graphene similar structures, has the electricity of excellence, light
The performances such as, magnetics, mechanics, can be applicable to different technical fields, thus become the focus of current material science research field
One of.Among numerous two-dimensional semiconductor materials, the sulfide ReS of rhenium (Re)2Be the most just be found have faint interlayer
Coupling and the two-dimensional semiconductor material of unique distortion 1T structure.The symmetry of lattice structure is the key factor determining material character
One of.Most of studied two-dimensional material all have high lattice symmetry, thus show isotropism.Reduce transition metal
In sulfide (TMDs) material, lattice symmetry can induce some anisotropy on Science and Technology with importance
Character.And rhenium disulfide (ReS2) inherently low-symmetry lattice material, therefore its electrical properties and optical property have respectively
Anisotropy.Due to rhenium disulfide (ReS2) there is the feature of faint layer coupling so that the rhenium disulfide (ReS of monolayer and multilamellar2)
Being all direct band gap, the change of the number of plies is to rhenium disulfide (ReS2) band structure almost not the biggest change, simply direct band gap
Size occurs in that faint change.The character of these uniquenesses allows rhenium disulfide (ReS2) scene effect transistor and photo-detector side
Mask has huge using value.
In the past few decades, possesses the physical and chemical performance of excellence and at following photoelectron due to nano material
Potential application in device, main attention is just concentrated in the preparation method research of nano material by research worker.
At present, the synthetic method of rhenium disulfide nanometer sheet has following report: T.Fujita etc. are entitled at document
《Chemically exfoliated ReS2Nanosheets " (" ReS prepared by chemical stripping method2Nanometer sheet ") middle employing chemistry
Lift-off technology has prepared rhenium disulfide nanometer sheet, and the method needs to carry out under inert gas shielding environment, and use
Lithium compound is the most inflammable, makes troubles to operation and dangerous.N.Al-Dulaimi etc. are entitled at document
《Sequential bottom-up and top-down processing for the synthesis of transition
metal dichalcogenide nanosheets:the case of rhenium disulfide(ReS2) " (" order is certainly
Descend and go up and process from top to bottom to synthesize transition metal dichalcogenide nanometer sheet: rhenium disulfide (ReS2) situation ") in use
Spraying assistant chemical vapor deposition and liquid phase peel off two kinds of technology, have prepared rhenium disulfide nanometer layer, and the method needs two steps
Operation, spraying assistant chemical vapor deposition needs high temperature, and technique is loaded down with trivial details.J.Gao etc. are at the entitled " Vertically of document
Oriented Arrays of ReS2Nanosheets for Electrochemical Energy Storage and
Electrocatalysis " (" ReS that the vertical orientation for electrochemical energy storage and electro-catalysis arranges2Nanometer sheet ") middle employingization
Learning gas phase deposition technology and prepared vertical orientated rhenium disulfide nanometer sheet, this process needs complicated control condition and high
Reaction temperature.Therefore, current low cost, rhenium disulfide nanometer sheet can be prepared on a large scale yet suffer from huge challenge.
Hydro-thermal method has been widely used for the preparation of nano material, and the principle of hydro-thermal method is to utilize air dry oven to reaction
System heating, pressurization, create high temperature, the environment of high pressure, thus carry out the preparation of material, compared with other preparation method,
Hydro-thermal method has following advantage: yield is high, can carry out large-scale production；Reaction condition is gentle, it is not necessary to the highest temperature；Atmosphere can
Control, it is not necessary to inert atmosphere；Technique is simple, low cost, it is not necessary to complicated instrument；Reactor is airtight, pollutes little.
Summary of the invention
In order to solve the problems referred to above, the invention provides a kind of side utilizing hydro-thermal reaction to prepare rhenium disulfide nanometer sheet
Method, the present invention is with ammonium perrhenate, oxammonium hydrochloride., thiourea as raw material, and water is solvent, during by regulation reaction temperature, hydro-thermal reaction
Between, thus prepare rhenium disulfide nanometer sheet.The present invention is simple to operate, it is not necessary to complicated reaction controlling condition, reaction temperature
Low, it is easy to large-scale production goes out high-quality rhenium disulfide nanometer sheet；Additionally, efficiency of the present invention is high, reproducible, low cost
Honest and clean, provide reliable sample preparation methods for rhenium disulfide nanometer sheet in the application of electrical and optical aspect.
The present invention is achieved through the following technical solutions:
A kind of method preparing rhenium disulfide nanometer sheet, specifically includes following steps:
Being 1: 1～5: 2～6 soluble in water by ammonium perrhenate, oxammonium hydrochloride., thiourea according to the amount ratio of material, preparation obtains
Ammonium perrhenate, oxammonium hydrochloride., thiourea total soluble matters substance withdrawl syndrome are the mixed solution of 0.1～0.4mol/L；By described mixing
Solution shifts in hydrothermal reaction kettle, and heating hydrothermal reaction kettle reaches reaction temperature and is incubated to maintain chemical reaction to carry out, preferably
Ground, reaction temperature is 160～260 DEG C, and the response time is 6～48 hours；After reaction terminates, hydrothermal reaction kettle temperature is cooled to
Room temperature, with water and ethanol, product cleaning in hydrothermal reaction kettle is clean, drying is final after processing prepares rhenium disulfide nanometer sheet.
Wherein, heating hydrothermal reaction kettle generally uses puts into baking oven for heating by hydrothermal reaction kettle, by regulation oven temperature
Regulate and control reaction temperature, by stop baking oven for heating hydrothermal reaction kettle and hydrothermal reaction kettle is cooled to room temperature terminate reaction,
Thus control the response time.
The present invention use ammonium perrhenate as rhenium source, thiourea as sulfur source, oxammonium hydrochloride. as reducing agent, oxammonium hydrochloride. and
Ammonium perrhenate reaction forms ReO42-, thiourea hydrolysis generates product and ReO42-Reaction forms rhenium disulfide nano-particle, at this
Under open fire heat condition, rhenium disulfide nano-particle assembles and forms rhenium disulfide nanometer sheet.The method have the advantages that behaviour
Making process simple, efficiency is high, reproducible, with low cost, can be prepared on a large scale out high-quality rhenium disulfide nanometer sheet；This
Bright provide reliable sample preparation methods for rhenium disulfide nanometer sheet in the application of electrical and optical aspect.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of rhenium disulfide nanometer sheet prepared by the present invention；
Fig. 2 is the Raman spectrogram of rhenium disulfide nanometer sheet prepared by the present invention；
Fig. 3 is the x-ray photoelectron energy spectrogram of rhenium disulfide nanometer sheet prepared by the present invention；
Fig. 4 is the transmission electron microscope figure of rhenium disulfide nanometer sheet prepared by the present invention.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with embodiment and Figure of description pair
The present invention is further elaborated:
Embodiment 1:
Weigh 0.5360 gram of ammonium perrhenate, 0.4170 gram of oxammonium hydrochloride. and 0.6850 gram of thiourea to be dissolved in 60 milliliters of water and stir
Mixing 30 minutes, prepared ammonium perrhenate, oxammonium hydrochloride., the total substance withdrawl syndrome of thiourea are the mixed solution of 0.28mol/L；By described
Mixed solution shifts in the hydrothermal reaction kettle inner bag of 100 milliliters, and then hydrothermal reaction kettle is put into the baking oven that temperature is 240 DEG C
In, it is incubated 24 hours to maintain chemical reaction to carry out；After reaction terminates, stop baking oven for heating, hydrothermal reaction kettle is taken out cooling
To room temperature, then with water and ethanol, product cleaning in hydrothermal reaction kettle is clean, it is dried under the conditions of 60 DEG C, final prepared two sulfur
Change rhenium nanometer sheet.
Fig. 1 is the X-ray diffractogram of rhenium disulfide nanometer sheet prepared by the present embodiment, the present embodiment as can be seen from Figure 1
The product of final synthesis is consistent with the standard PDF card of rhenium disulfide, belongs to anorthic system, and therefore prepared by the embodiment of the present invention
Go out rhenium disulfide nanometer sheet.
Embodiment 2:
Weigh 0.5360 gram of ammonium perrhenate, 0.1040 gram of oxammonium hydrochloride. and 0.3045 gram of thiourea to be dissolved in 60 milliliters of water and stir
Mixing 30 minutes, prepared ammonium perrhenate, oxammonium hydrochloride., the total substance withdrawl syndrome of thiourea are the mixed solution of 0.13mol/L；By described
Mixed solution shifts in the hydrothermal reaction kettle inner bag of 100 milliliters, and then hydrothermal reaction kettle is put into the baking oven that temperature is 240 DEG C
In, it is incubated 6 hours to maintain chemical reaction to carry out；After reaction terminates, stop baking oven for heating, hydrothermal reaction kettle is taken out and is cooled to
Room temperature, then with water and ethanol, product cleaning in hydrothermal reaction kettle is clean, it is dried under the conditions of 60 DEG C, finally prepares curing
Rhenium nanometer sheet.
Fig. 2 is the Raman spectrogram of rhenium disulfide nanometer sheet prepared by the present embodiment, as can be seen from Figure 2 exists
161.7cm-1And 211.4cm-1Two Characteristic Raman peaks of rhenium disulfide occur.
Embodiment 3:
Weigh 0.5360 gram of ammonium perrhenate, 0.6950 gram of oxammonium hydrochloride. and 0.7612 gram of thiourea to be dissolved in 60 milliliters of water and stir
Mixing 30 minutes, prepared ammonium perrhenate, oxammonium hydrochloride., the total substance withdrawl syndrome of thiourea are the mixed solution of 0.37mol/L；By described
Mixed solution shifts in the hydrothermal reaction kettle inner bag of 100 milliliters, and then hydrothermal reaction kettle is put into the baking oven that temperature is 160 DEG C
In, it is incubated 24 hours to maintain chemical reaction to carry out；After reaction terminates, stop baking oven for heating, hydrothermal reaction kettle is taken out cooling
To room temperature, then with water and ethanol, product cleaning in hydrothermal reaction kettle is clean, it is dried under the conditions of 60 DEG C, final prepared two sulfur
Change rhenium nanometer sheet.
Fig. 3 is the x-ray photoelectron energy spectrogram of rhenium disulfide prepared by the embodiment of the present invention, from figure (a) it can be seen that Re
The 4f valence state of atom, at 42.2eV and 44.6eV, corresponds respectively to the 4f of Re atom7/2Track and the 4f of Re atom5/2Track,
From figure (b) it can be seen that the 2p of S atom3/2Track and the 2p of S atom1/2Track occurs at 162.5eV and 163.7eV, therefore
It is consistent with rhenium disulfide crystal corresponding parametric values.
Embodiment 4:
Weigh 0.5360 gram of ammonium perrhenate, 0.4170 gram of oxammonium hydrochloride. and 0.6850 gram of thiourea to be dissolved in 60 milliliters of water and stir
Mixing 30 minutes, prepared ammonium perrhenate, oxammonium hydrochloride., the total substance withdrawl syndrome of thiourea are the mixed solution of 0.28mol/L；By described
Mixed solution shifts in the hydrothermal reaction kettle inner bag of 100 milliliters, and then hydrothermal reaction kettle is put into the baking oven that temperature is 260 DEG C
In, it is incubated 48 hours to maintain chemical reaction to carry out；After reaction terminates, stop baking oven for heating, hydrothermal reaction kettle is taken out cooling
To room temperature, then with water and ethanol, product cleaning in hydrothermal reaction kettle is clean, it is dried under the conditions of 60 DEG C, final prepared two sulfur
Change rhenium nanometer sheet.
Fig. 4 is the transmission electron microscope photo of rhenium disulfide prepared by the present embodiment, from Fig. 4 it can be clearly seen that two
Sulfuration rhenium nanometer sheet, the lattice fringe spacing in figure is 0.61nm, corresponding to (100) crystal face of rhenium disulfide.
The principle of above-described embodiment only illustrative present invention and effect thereof, not for limiting the present invention.Any ripe
Above-described embodiment all can be modified under the spirit and the scope of the present invention or change by the personage knowing this technology.Cause
This, have usually intellectual such as complete with institute under technological thought without departing from disclosed spirit in art
All equivalences become are modified or change, and must be contained by the claim of the present invention.
Claims (4)
1. the method preparing rhenium disulfide nanometer sheet, it is characterised in that comprise the following steps: by ammonium perrhenate, hydrochloric acid hydroxyl
Amine, thiourea are 1: 1～5: 2～6 soluble in water according to the amount ratio of material, and preparation obtains ammonium perrhenate, oxammonium hydrochloride., the total thing of thiourea
The mixed solution that amount concentration is 0.1～0.4mol/L of matter, shifts in hydrothermal reaction kettle by described mixed solution, adds hot water thermal
Reactor reaches reaction temperature and is incubated to maintain the carrying out of chemical reaction, after reaction terminates, hydrothermal reaction kettle temperature is cooled to
Room temperature, with water and ethanol by product cleaning in hydrothermal reaction kettle, drying is final after processing prepares rhenium disulfide nanometer sheet.
A kind of method preparing rhenium disulfide nanometer sheet the most according to claim 1, it is characterised in that hydrothermal reaction kettle leads to
Cross baking oven for heating.
A kind of method preparing rhenium disulfide nanometer sheet the most according to claim 1 and 2, it is characterised in that described reaction
Temperature is 160～260 DEG C.
A kind of method preparing rhenium disulfide nanometer sheet the most according to claim 1 and 2, it is characterised in that response time
It it is 6～48 hours.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107362812A (en) * | 2017-07-25 | 2017-11-21 | 苏州大学 | A kind of compound two-dimensional material of selenium sulfuration rhenium, preparation method and applications |
| CN108483502A (en) * | 2018-06-05 | 2018-09-04 | 中南大学 | A kind of preparation method and application of rhenium disulfide nanometer sheet |
| CN109546098A (en) * | 2018-10-11 | 2019-03-29 | 天津大学 | The preparation method of redox graphene load ReS2 for lithium sulfur battery anode material |
| CN109545573A (en) * | 2018-03-21 | 2019-03-29 | 信阳学院 | The preparation method of metal 1T phase sulfuration rhenium hollow nanospheres electrode material for super capacitor |
| CN110002504A (en) * | 2019-04-30 | 2019-07-12 | 陕西科技大学 | A kind of preparation method of rhenium disulfide nanometer sheet |
| CN110061204A (en) * | 2019-03-21 | 2019-07-26 | 天津大学 | Two-dimensional honeycomb carbon nanosheet coated 1T' -ReS2Preparation method of sodium ion battery cathode material |
| CN110143616A (en) * | 2019-04-30 | 2019-08-20 | 陕西科技大学 | A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth |
| CN110508292A (en) * | 2019-07-15 | 2019-11-29 | 天津大学 | The preparation method of metal-doped rhenium disulfide nano-chip arrays for electro-catalysis complete solution water |
| CN110538662A (en) * | 2019-07-01 | 2019-12-06 | 天津大学 | Preparation method of cobalt-doped rhenium disulfide nanosheet array for electrocatalytic hydrogen evolution |
| CN110838586A (en) * | 2018-08-15 | 2020-02-25 | 深圳国家能源新材料技术研发中心有限公司 | Rhenium sulfide nanotube and preparation method and application thereof |
| CN110838572A (en) * | 2018-08-15 | 2020-02-25 | 深圳国家能源新材料技术研发中心有限公司 | Nano composite material and preparation method and application thereof |
| CN111072069A (en) * | 2019-09-25 | 2020-04-28 | 江南大学 | Method for preparing visible light response 2D rhenium disulfide and application |
| CN111170370A (en) * | 2020-01-19 | 2020-05-19 | 华南师范大学 | Manufacturing method of rhenium disulfide supercapacitor based on biological template growth |
| CN111354935A (en) * | 2020-03-24 | 2020-06-30 | 东华大学 | Defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material and preparation method thereof |
| CN112018351A (en) * | 2020-08-13 | 2020-12-01 | 五邑大学 | Nano ReS2Mxene composite material and preparation method thereof |
| CN116495789A (en) * | 2023-04-24 | 2023-07-28 | 闽都创新实验室 | Preparation method and application of ultrathin rhenium sulfide nanosheets |
| CN116495789B (en) * | 2023-04-24 | 2024-04-30 | 闽都创新实验室 | Preparation method and application of ultrathin rhenium sulfide nanosheets |
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Cited By (23)
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| CN107362812A (en) * | 2017-07-25 | 2017-11-21 | 苏州大学 | A kind of compound two-dimensional material of selenium sulfuration rhenium, preparation method and applications |
| CN107362812B (en) * | 2017-07-25 | 2019-10-22 | 苏州大学 | A kind of compound two-dimensional material of selenium sulfuration rhenium, preparation method and applications |
| CN109545573A (en) * | 2018-03-21 | 2019-03-29 | 信阳学院 | The preparation method of metal 1T phase sulfuration rhenium hollow nanospheres electrode material for super capacitor |
| CN109545573B (en) * | 2018-03-21 | 2020-08-28 | 信阳学院 | Preparation method of metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material |
| CN108483502A (en) * | 2018-06-05 | 2018-09-04 | 中南大学 | A kind of preparation method and application of rhenium disulfide nanometer sheet |
| CN108483502B (en) * | 2018-06-05 | 2020-05-19 | 中南大学 | Preparation method and application of rhenium disulfide nanosheet |
| CN110838586A (en) * | 2018-08-15 | 2020-02-25 | 深圳国家能源新材料技术研发中心有限公司 | Rhenium sulfide nanotube and preparation method and application thereof |
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| CN109546098A (en) * | 2018-10-11 | 2019-03-29 | 天津大学 | The preparation method of redox graphene load ReS2 for lithium sulfur battery anode material |
| CN110061204A (en) * | 2019-03-21 | 2019-07-26 | 天津大学 | Two-dimensional honeycomb carbon nanosheet coated 1T' -ReS2Preparation method of sodium ion battery cathode material |
| CN110061204B (en) * | 2019-03-21 | 2022-03-29 | 天津大学 | Two-dimensional honeycomb carbon nanosheet coated 1T' -ReS2Preparation method of sodium ion battery cathode material |
| CN110002504A (en) * | 2019-04-30 | 2019-07-12 | 陕西科技大学 | A kind of preparation method of rhenium disulfide nanometer sheet |
| CN110143616A (en) * | 2019-04-30 | 2019-08-20 | 陕西科技大学 | A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth |
| CN110002504B (en) * | 2019-04-30 | 2021-04-27 | 陕西科技大学 | Preparation method of rhenium disulfide nanosheet |
| CN110143616B (en) * | 2019-04-30 | 2021-05-28 | 陕西科技大学 | Preparation method of vertically-grown rhenium disulfide nanosheet |
| CN110538662A (en) * | 2019-07-01 | 2019-12-06 | 天津大学 | Preparation method of cobalt-doped rhenium disulfide nanosheet array for electrocatalytic hydrogen evolution |
| CN110508292A (en) * | 2019-07-15 | 2019-11-29 | 天津大学 | The preparation method of metal-doped rhenium disulfide nano-chip arrays for electro-catalysis complete solution water |
| CN111072069A (en) * | 2019-09-25 | 2020-04-28 | 江南大学 | Method for preparing visible light response 2D rhenium disulfide and application |
| CN111170370A (en) * | 2020-01-19 | 2020-05-19 | 华南师范大学 | Manufacturing method of rhenium disulfide supercapacitor based on biological template growth |
| CN111354935A (en) * | 2020-03-24 | 2020-06-30 | 东华大学 | Defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material and preparation method thereof |
| CN112018351A (en) * | 2020-08-13 | 2020-12-01 | 五邑大学 | Nano ReS2Mxene composite material and preparation method thereof |
| CN116495789A (en) * | 2023-04-24 | 2023-07-28 | 闽都创新实验室 | Preparation method and application of ultrathin rhenium sulfide nanosheets |
| CN116495789B (en) * | 2023-04-24 | 2024-04-30 | 闽都创新实验室 | Preparation method and application of ultrathin rhenium sulfide nanosheets |
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