CN106379871A - Method for preparing rhenium diselenide nano-sheet - Google Patents
Method for preparing rhenium diselenide nano-sheet Download PDFInfo
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- CN106379871A CN106379871A CN201610887905.4A CN201610887905A CN106379871A CN 106379871 A CN106379871 A CN 106379871A CN 201610887905 A CN201610887905 A CN 201610887905A CN 106379871 A CN106379871 A CN 106379871A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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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
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
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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
- C01P2002/70—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
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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 a rhenium diselenide nano-sheet and belongs to the field of preparation of a novel two-dimensional nano material. The rhenium diselenide nano-sheet is formed through reducing a rhenium source and a selenium source through hydroxylammonium chloride by utilizing a hydrothermal method, reacting to obtain rhenium diselenide nano-particles and assembling the rhenium diselenide nano-particles. By adopting the method provided by the invention, the disadvantages of an existing preparation process of the rhenium diselenide nano-sheet that a preparation period is long, the cost is high, the operation is complicated and the like are overcome; the method is simple in production operation and good in repeatability and a reaction period is shortened; raw materials for producing are cheap and easy to obtain; the method has moderate reaction conditions, and energy consumption and cost are reduced, so that the method is suitable for large-scale production; the invention provides a reliable sample preparation method for application of the rhenium diselenide nano-sheet in electrical and optical aspects, and provides more potential scientific evidences and technical supports for enabling the rhenium diselenide nano-sheet to become a novel photoelectric material in the future.
Description
Technical field
The invention belongs to New Two Dimensional field of nano material preparation is and in particular to a kind of side preparing two selenizing rhenium nanometer sheet
Method.
Background technology
Transient metal chalcogenide compound (TMDs) material is a kind of two-dimensional semiconductor electricity of emerging, similar graphene-structured
Sub- material.Wherein, metal sulfide, selenides are important semi-conducting materials, and nano metal sulphide, selenide material have
Special nonlinear optical property, good luminescence generated by light and electroluminescence characters, significant quantum size effect, catalysis, storage
Can etc. important physicochemical properties, can be widely applied to various light-emitting devices, laser detector, nonlinear optical material,
Sensing material etc..
Among numerous two-dimensional semiconductor materials, the chalcogenide ReS of rhenium (Re)2And ReSe2It is just to be found recently
The two-dimensional semiconductor material having faint layer coupling and unique distortion 1T structure.The symmetry of lattice structure is to determine material
One of key factor of matter.Most of studied two-dimensional material all have high lattice symmetry, thus showing isotropism.
Therefore, reduce lattice symmetry in transient metal chalcogenide compound (TMDs) material and can induce some on Science and Technology
There are the anisotropic properties of importance.And two selenizing rhenium (ReSe2) inherently low-symmetry lattice material, therefore its electricity
Property and optical property have anisotropy.Due to two selenizing rhenium (ReSe2) there is faint layer coupling so that monolayer
And two selenizing rhenium (ReSe of multilamellar2) it is all direct band gap, the change of the number of plies is to two selenizing rhenium (ReSe2) band structure almost
Do not have too big change, simply the size of direct band gap occurs in that faint change.These unique properties above-mentioned allow two selenizing rheniums
(ReSe2) aspect such as scene effect transistor and photo-detector has huge using value.
In the past few decades, because nano material possesses excellent physical and chemical performance and its in following photoelectron
Potential application in device, research worker just concentrates on main attention in the preparation method research of nano material.At present, two selenium
The synthetic method changing rhenium nanometer sheet has following report:
B.Jariwala etc. is entitled in document《Synthesis and Characterization of ReS2and
ReSe2Layered Chalcogenide Single Crystals》(《Synthesis and sign ReS2And ReSe2Stratiform chalkogenide
Monocrystalline》) in disclose and adopt improved Bridgman method so that two selenizing rhenium monocrystalline are obtained, however, the method needs low true
Carry out under sky and hot environment, reaction time is extremely long, make troubles to operation and dangerous;M.Hafeez etc. is entitled in document
《Chemical Vapor Deposition Synthesis of Ultrathin Hexagonal ReSe2Flakes for
Anisotropic Raman Property and Optoelectronic Application》(《Chemical vapor deposition synthesizes
The anisotropic Raman property of ultra-thin ReSe2 piece and photovoltaic applications》) in provide and a kind of adopt chemical vapour deposition technique system
Method for going out two selenizing rhenium nanometer sheet, this process needs complicated control condition and higher reaction temperature;D.B.Seley etc.
Entitled in document《ReSe2nanotubes synthesized from sacrificial templates》(《Using sacrifice
Templated synthesis ReSe2Nanotube》) in disclose a kind of method preparing two selenizing rhenium nanotubes using solvent thermal technology,
The method needs to be divided into two step operations, and reaction time is long, and technique is loaded down with trivial details.
In sum, the preparation of current two selenizing rhenium nanometer sheet yet suffers from long preparation period, high cost, complex operation etc.
Problem is it is impossible to realize extensive, technology production, therefore, the large-scale production of two selenizing rhenium nanometer sheet faces huge challenge.
Content of the invention
In view of mentioned above, the defect existing for the existing stage and deficiency, the present invention provides one kind to prepare two selenizing rheniums
The method of nanometer sheet, the method is that rhenium source and selenium source are utilized the reduction through oxammonium hydrochloride. for the hydro-thermal method, and reaction obtains two selenizing rheniums
Nano-particle, and then assemble formation two selenizing rhenium nanometer sheet.
The present invention adopts the following technical scheme that:
A kind of method preparing two selenizing rhenium nanometer sheet, comprises the following steps:
Step A:By ammonium perrhenate, oxammonium hydrochloride., selenium source according to ammonium perrhenate: oxammonium hydrochloride.: the ratio of selenium source is 10mol: 1
The ratio of~60mol: 20~50mol is dissolved in the water, and prepares the amount of the total material obtaining ammonium perrhenate, oxammonium hydrochloride. and selenium source
Concentration is the homogeneous mixture solotion of 0.1~0.4mol/L;
Step B:The mixed solution of step A gained is shifted in hydrothermal reaction kettle, heating hydrothermal reaction kettle reaches reaction temperature
Spend and be incubated to maintain the carrying out of chemical reaction, after reaction terminates, hydrothermal reaction kettle temperature is cooled to room temperature, separates and obtain water
Hot;
Step C:Step B gained hydrothermal product water and ethanol are carried out, drying is finally obtained two selenium after processing
Change rhenium nanometer sheet.
In the present invention, described selenium source can be Monohydrated selenium dioxide, selenite or selenium dioxide;
Further, in step B of the present invention, reaction temperature is 180~260 DEG C.
Further, in step B of the present invention, the response time is 6~48 hours.
The present invention participates in the rhenium source of reaction, selenium source and oxammonium hydrochloride. are that analysis is pure, and the present invention adopts ammonium perrhenate conduct
Rhenium source, as selenium source, oxammonium hydrochloride. is as reducing agent, oxammonium hydrochloride. and ammonium perrhenate for Monohydrated selenium dioxide, selenite or selenium dioxide
Reaction forms ReO4 2-, selenium source hydrolysis generates product and ReO4 2-Reaction forms two selenizing rhenium nano-particle, according to hydro-thermal of the present invention
Condition, two selenizing rhenium nano-particle assemblings form two selenizing rhenium nanometer sheet.
Compared to existing technology, beneficial effects of the present invention are as follows:The present invention is simple to operate, favorable reproducibility, shortens reaction week
Phase;Selenium source used, rhenium source are all cheap and easy to get, and because the reaction condition of the method is gentle, decreases energy consumption and cost, be conducive to
Large-scale production;The present invention is that two selenizing rhenium nanometer sheet provide reliable sample preparation side in the application of electrical and optical aspect
Method.
Brief description
The X-ray diffractogram of the two selenizing rhenium nanometer sheet that Fig. 1 is prepared for the present invention;
The Raman spectrogram of the two selenizing rhenium nanometer sheet that Fig. 2 is prepared for the present invention;
The x-ray photoelectron energy spectrum diagram of the two selenizing rhenium nanometer sheet that Fig. 3 is prepared for the present invention;
The transmission electron microscope figure of the two selenizing rhenium nanometer sheet that Fig. 4 is prepared for the present invention;
The scanning electron microscope diagram of the two selenizing rhenium nanometer sheet that Fig. 5 is prepared for the present invention.
Specific embodiment
The present invention will be described in more detail with Figure of description with reference to embodiments:
Embodiment 1:
A kind of method preparing two selenizing rhenium nanometer sheet, comprises the following steps:
Step A:0.5365 gram of ammonium perrhenate, 0.1390 gram of oxammonium hydrochloride. and 0.6450 gram of Monohydrated selenium dioxide are dissolved in 60ml water
In, stir 30 minutes, the amount concentration preparing the total material obtaining ammonium perrhenate, oxammonium hydrochloride. and Monohydrated selenium dioxide is 0.15mol/L's
Homogeneous mixture solotion;
Step B:The mixed solution of step A gained is shifted in 80ml hydrothermal reaction kettle inner bag, then by hydro-thermal reaction
Kettle is placed in heating in 240 DEG C of baking ovens, 24 hours carrying out with maintenance chemical reaction of insulation;After reaction terminates, by hydrothermal reaction kettle
It is cooled to room temperature after taking-up, separate and obtain hydrothermal product;
Step C:Step B gained hydrothermal product water and ethanol are carried out, dried under the conditions of 60 DEG C, finally
Two selenizing rhenium nanometer sheet are obtained.
Fig. 1 is the X-ray diffractogram of two selenizing rhenium nanometer sheet manufactured in the present embodiment, it will be seen from figure 1 that the present embodiment
The product of final synthesis is consistent with the standard PDF card of two selenizing rheniums, belongs to anorthic system, shows embodiment of the present invention gained
Product is two selenizing rhenium nanometer sheet.
Embodiment 2:
A kind of method preparing two selenizing rhenium nanometer sheet, comprises the following steps:
Step A:0.5365 gram of ammonium perrhenate, 0.1390 gram of oxammonium hydrochloride. and 0.4438 gram of selenium dioxide are dissolved in 60ml
In water, stir 30 minutes, the amount concentration preparing the total material obtaining ammonium perrhenate, oxammonium hydrochloride. and Monohydrated selenium dioxide is 0.10mol/L
Homogeneous mixture solotion;
Step B:The mixed solution of step A gained is shifted in 80ml hydrothermal reaction kettle inner bag, then by hydro-thermal reaction
Kettle is placed in heating in 240 DEG C of baking ovens, 24 hours carrying out with maintenance chemical reaction of insulation;After reaction terminates, by hydrothermal reaction kettle
It is cooled to room temperature after taking-up, separate and obtain hydrothermal product;
Step C:Step B gained hydrothermal product water and ethanol are carried out, dried under the conditions of 60 DEG C, finally
Two selenizing rhenium nanometer sheet are obtained.
Fig. 2 is the Raman spectrogram of two selenizing rhenium nanometer sheet manufactured in the present embodiment, from figure 2 it can be seen that
124cm-1And 174cm-1Occur in that two Characteristic Raman peaks of two selenizing rheniums at position, show that the embodiment of the present invention is obtained two selenium
Change rhenium nanometer sheet.
Embodiment 3:
A kind of method preparing two selenizing rhenium nanometer sheet, comprises the following steps:
Step A:0.5365 gram of ammonium perrhenate, 0.6949 gram of oxammonium hydrochloride. and 1.0318 grams of Monohydrated selenium dioxides are dissolved in 60ml water
In, stir 30 minutes, the amount concentration preparing the total material obtaining ammonium perrhenate, oxammonium hydrochloride. and Monohydrated selenium dioxide is 0.33mol/L's
Homogeneous mixture solotion;
Step B:The mixed solution of step A gained is shifted in 80ml hydrothermal reaction kettle inner bag, then by hydro-thermal reaction
Kettle is placed in heating in 180 DEG C of baking ovens, 24 hours carrying out with maintenance chemical reaction of insulation;After reaction terminates, by hydrothermal reaction kettle
It is cooled to room temperature after taking-up, separate and obtain hydrothermal product;
Step C:Step B gained hydrothermal product water and ethanol are carried out, dried under the conditions of 60 DEG C, finally
Two selenizing rhenium nanometer sheet are obtained.
The x-ray photoelectron energy spectrum diagram of the two selenizing rheniums that Fig. 3 is prepared for the embodiment of the present invention, can be seen that from figure (a):Re
4f valence state, at 41.7eV and 44.1eV, corresponds respectively to Re 4f7/2Track and Re 4f5/2Track, can be seen that from figure (b):
Se 3d5/2Track and Se 3d3/2Track at 54.7eV and 55.6eV, these numerical value and two selenizing rhenium crystal relevant parameters
Value is consistent.
Embodiment 4:
A kind of method preparing two selenizing rhenium nanometer sheet, comprises the following steps:
Step A:0.5365 gram of ammonium perrhenate, 0.2780 gram of oxammonium hydrochloride. and 0.6449 gram of Monohydrated selenium dioxide are dissolved in 60ml water
In, stir 30 minutes, the amount concentration preparing the total material obtaining ammonium perrhenate, oxammonium hydrochloride. and Monohydrated selenium dioxide is 0.18mol/L's
Homogeneous mixture solotion;
Step B:The mixed solution of step A gained is shifted in 80ml hydrothermal reaction kettle inner bag, then by hydro-thermal reaction
Kettle is placed in heating in 260 DEG C of baking ovens, 6 hours carrying out with maintenance chemical reaction of insulation;After reaction terminates, hydrothermal reaction kettle is taken
It is cooled to room temperature after going out, separate and obtain hydrothermal product;
Step C:Step B gained hydrothermal product water and ethanol are carried out, dried under the conditions of 60 DEG C, finally
Two selenizing rhenium nanometer sheet are obtained.
Fig. 4 is the transmission electron microscope figure of two selenizing rheniums manufactured in the present embodiment, can be clearly seen that two selenium from Fig. 4
Change rhenium nanometer sheet, the lattice fringe spacing in Fig. 4 is 0.64nm, corresponding to (001) crystal face of two selenizing rheniums.
Embodiment 5:
A kind of method preparing two selenizing rhenium nanometer sheet, comprises the following steps:
Step A:0.5365 gram of ammonium perrhenate, 0.1390 gram of oxammonium hydrochloride. and 0.8647 gram of sodium selenite are dissolved in 60ml
In water, stir 30 minutes, the amount concentration preparing the total material obtaining ammonium perrhenate, oxammonium hydrochloride. and sodium selenite is 0.15mol/
The homogeneous mixture solotion of L;
Step B:The mixed solution of step A gained is shifted in 80ml hydrothermal reaction kettle inner bag, then by hydro-thermal reaction
Kettle is placed in heating in 220 DEG C of baking ovens, 48 hours carrying out with maintenance chemical reaction of insulation;After reaction terminates, by hydrothermal reaction kettle
It is cooled to room temperature after taking-up, separate and obtain hydrothermal product;
Step C:Step B gained hydrothermal product water and ethanol are carried out, dried under the conditions of 60 DEG C, finally
Two selenizing rhenium nanometer sheet are obtained.
Fig. 5 is the electron scanning micrograph of two selenizing rheniums manufactured in the present embodiment, can be clearly seen that two from Fig. 5
The microscopic appearance of selenizing rhenium nanometer sheet.
Above-described embodiment only principle of the illustrative present invention and its effect, not for the restriction present invention.Any ripe
The personage knowing this technology all can carry out modifications and changes without prejudice under the spirit and the scope of the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
All equivalent modifications becoming or change, must be covered by the claim of the present invention.
Claims (4)
1. a kind of method preparing two selenizing rhenium nanometer sheet is it is characterised in that comprise the following steps:
Step A:By ammonium perrhenate, oxammonium hydrochloride. and selenium source according to ammonium perrhenate: oxammonium hydrochloride.: the amount of the material of selenium source is than for 10
: 1~60: 20~50 ratio is dissolved in the water, and prepares the amount concentration of the total material obtaining ammonium perrhenate, oxammonium hydrochloride. and selenium source
Homogeneous mixture solotion for 0.1~0.4mol/L;
Step B:The mixed solution of step A gained is shifted in hydrothermal reaction kettle, heating hydrothermal reaction kettle reaches reaction temperature simultaneously
Insulation, to maintain the carrying out of chemical reaction, after reaction terminates, hydrothermal reaction kettle temperature is cooled to room temperature, separates and obtains hydro-thermal product
Thing;
Step C:Step B gained hydrothermal product water and ethanol are carried out, drying is finally obtained two selenizing rheniums after processing
Nanometer sheet.
2. a kind of method preparing two selenizing rhenium nanometer sheet according to claim 1 is it is characterised in that in described step B
Reaction temperature is 180~260 DEG C.
3. a kind of method preparing two selenizing rhenium nanometer sheet according to claim 2 is it is characterised in that in described step B
It is incubated with the time maintaining chemical reaction for 6~48 hours.
4. a kind of method preparing two selenizing rhenium nanometer sheet according to claim 1 is it is characterised in that described selenium source is Asia
Selenic acid, selenite or selenium dioxide.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
CN108862397A (en) * | 2018-06-15 | 2018-11-23 | 肇庆市华师大光电产业研究院 | A kind of method directly growing uniform two selenizings rhenium nanometer sheet on basal electrode and modified electrode and application |
CN111318288A (en) * | 2020-03-25 | 2020-06-23 | 江南大学 | Rhenium diselenide/carbon nanofiber composite electrocatalytic material and preparation method thereof |
CN111389420A (en) * | 2020-03-25 | 2020-07-10 | 江南大学 | Vacancy-rich rhenium diselenide-based multi-level hydrophobic film and preparation method thereof |
CN113501504A (en) * | 2021-07-21 | 2021-10-15 | 苏州普轮电子科技有限公司 | Novel semiconductor material with micro-nano structure and preparation method thereof |
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Cited By (6)
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 |
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 |
CN108862397A (en) * | 2018-06-15 | 2018-11-23 | 肇庆市华师大光电产业研究院 | A kind of method directly growing uniform two selenizings rhenium nanometer sheet on basal electrode and modified electrode and application |
CN111318288A (en) * | 2020-03-25 | 2020-06-23 | 江南大学 | Rhenium diselenide/carbon nanofiber composite electrocatalytic material and preparation method thereof |
CN111389420A (en) * | 2020-03-25 | 2020-07-10 | 江南大学 | Vacancy-rich rhenium diselenide-based multi-level hydrophobic film and preparation method thereof |
CN113501504A (en) * | 2021-07-21 | 2021-10-15 | 苏州普轮电子科技有限公司 | Novel semiconductor material with micro-nano structure and preparation method thereof |
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