CN106379871B - A kind of method for preparing two selenizing rhenium nanometer sheets - Google Patents
A kind of method for preparing two selenizing rhenium nanometer sheets Download PDFInfo
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- CN106379871B CN106379871B CN201610887905.4A CN201610887905A CN106379871B CN 106379871 B CN106379871 B CN 106379871B CN 201610887905 A CN201610887905 A CN 201610887905A CN 106379871 B CN106379871 B CN 106379871B
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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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- 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 kind of method for preparing two selenizing rhenium nanometer sheets, belong to New Two Dimensional field of nano material preparation.The present invention reduces in rhenium source and selenium source using hydro-thermal method through hydroxylamine hydrochloride, and reaction obtains two selenizing rhenium nano particles, and then assembles and form two selenizing rhenium nanometer sheets.The present invention overcomes the long preparation period present in the two existing preparation processes of selenizing rhenium nanometer sheet, it is of high cost, complicated the shortcomings of, production operation of the present invention is simple, favorable reproducibility, shorten reaction time；Raw materials for production are cheap and easy to get, and since the reaction condition of this method is gentle, reduce energy consumption and cost, are conducive to mass produce；The present invention provides reliable sample preparation methods for application of the two selenizing rhenium nanometer sheets at electrical and optical aspect, and becoming following novel photoelectric material for it provides more potential scientific basis and technical support.
Description
Technical field
The invention belongs to New Two Dimensional field of nano material preparation, and in particular to a kind of side for preparing two selenizing rhenium nanometer sheets
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 for having faint layer coupling and unique distortion 1T structures.The symmetry of lattice structure is to determine material
One of an important factor for matter.Most of studied two-dimensional materials all have high lattice symmetry, so as to show isotropism.
Therefore, some can be induced on Science and Technology by reducing lattice symmetry in transient metal chalcogenide compound (TMDs) material
Anisotropic properties with 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 individual layer
And two selenizing rhenium (ReSe of multilayer2) all it is direct band gap, the change of the number of plies is to two selenizing rhenium (ReSe2) band structure almost
There is faint change in too not big change, the size for being direct band gap.These above-mentioned unique properties allow two selenizing rheniums
(ReSe2) scene effect transistor and optical detector etc. have huge application value.
In the past few decades, since nano material possesses excellent physical and chemical performance and its in following photoelectron
Potential application in device, researcher just concentrate on main attention in the preparation method research of nano material.At present, two selenium
The synthetic method for changing rhenium nanometer sheet has following report：
B.Jariwala etc. is entitled in document《Synthesis and Characterization of ReS2 and
ReSe2Layered Chalcogenide Single Crystals》(《Synthesis and characterization ReS2And ReSe2Stratiform chalkogenide
Monocrystalline》) in disclose and use improved Bridgman methods so that two selenizing rhenium monocrystalline are made, however, this method is needed low true
Carried out under empty and hot environment, reaction time is extremely long, makes troubles to operation and dangerous；M.Hafeez etc. is entitled in document
《Chemical Vapor Deposition Synthesis of Ultrathin Hexagonal ReSe2 Flakes for
Anisotropic Raman Property and Optoelectronic Application》(《Chemical vapor deposition synthesizes
Anisotropic the Raman property and photovoltaic applications of ultra-thin ReSe2 pieces》) in provide and a kind of use chemical vapour deposition technique system
For the method for going out two selenizing rhenium nanometer sheets, which needs complicated control condition and higher reaction temperature；D.B.Seley etc.
It is entitled in document《ReSe2nanotubes synthesized from sacrificial templates》(《Utilize sacrifice
Templated synthesis ReSe2Nanotube》) in disclose it is a kind of using solvent thermal technology to prepare the method for two selenizing rhenium nanotubes,
This method needs to be divided into the operation of two steps, grows reaction time, technique is cumbersome.
In conclusion the preparation of current two selenizings rhenium nanometer sheet still has long preparation period, and it is of high cost, it is complicated etc.
Problem, can not realize extensive, technology production, therefore, the large-scale production of two selenizing rhenium nanometer sheets faces huge challenge.
The content of the invention
In view of described above, for the existing stage there are the defects of and deficiency, the present invention one kind is provided and prepares two selenizing rheniums
The method of nanometer sheet, this method are that rhenium source and selenium source are utilized reduction of the hydro-thermal method through hydroxylamine hydrochloride, and reaction obtains two selenizing rheniums
Nano particle, and then assemble and form two selenizing rhenium nanometer sheets.
The present invention adopts the following technical scheme that：
A kind of method for preparing two selenizing rhenium nanometer sheets, comprises the following steps：
Step A：By ammonium perrhenate, hydroxylamine hydrochloride, selenium source according to ammonium perrhenate: hydroxylamine hydrochloride: the ratio of selenium source is 10mol: 1
The ratio of~60mol: 20~50mol is dissolved in the water, and prepares the amount for the total material for obtaining ammonium perrhenate, hydroxylamine hydrochloride and selenium source
Concentration is the homogeneous mixture solotion of 0.1~0.4mol/L；
Step B：Mixed solution obtained by step A is shifted in hydrothermal reaction kettle, heating hydrothermal reaction kettle is warm up to reaction
Spend and keep the temperature to maintain the progress of chemical reaction, after reaction, hydrothermal reaction kettle temperature is cooled to room temperature, isolated water
Hot；
Step C：Hydrothermal product obtained by step B is cleaned with water and alcohol, two selenium are finally made after drying process
Change rhenium nanometer sheet.
In the present invention, the selenium source can be selenous acid, selenite or selenium dioxide；
Further, reaction temperature is 180~260 DEG C in step B of the present invention.
Further, when the reaction time is 6~48 small in step B of the present invention.
Rhenium source, selenium source and the hydroxylamine hydrochloride that the present invention participates in reaction are that analysis is pure, and the present invention uses ammonium perrhenate conduct
Rhenium source, selenous acid, selenite or selenium dioxide are as selenium source, and hydroxylamine hydrochloride is as reducing agent, hydroxylamine hydrochloride and ammonium perrhenate
Reaction forms ReO4 2-, selenium source, which hydrolyzes, generates product and ReO4 2-Reaction forms two selenizing rhenium nano particles, according to hydro-thermal of the present invention
Condition, two selenizing rhenium nano particles assemble to form two selenizing rhenium nanometer sheets.
Compared with prior art, beneficial effects of the present invention are as follows：Easy to operate, favorable reproducibility of the invention, shortens reaction week
Phase；Selenium source used, rhenium source are cheap and easy to get, and since the reaction condition of this method is gentle, reduces energy consumption and cost, be conducive to
Large-scale production；The present invention provides reliable sample preparation side for application of the two selenizing rhenium nanometer sheets at electrical and optical aspect
Method.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of two selenizing rhenium nanometer sheets prepared by the present invention；
Fig. 2 is the Raman spectrogram of two selenizing rhenium nanometer sheets prepared by the present invention；
Fig. 3 is the x-ray photoelectron spectroscopy figure of two selenizing rhenium nanometer sheets prepared by the present invention；
Fig. 4 is the transmission electron microscope figure of two selenizing rhenium nanometer sheets prepared by the present invention；
Fig. 5 is the scanning electron microscope diagram of two selenizing rhenium nanometer sheets prepared by the present invention.
Embodiment
The present invention will be described in more detail with Figure of description with reference to embodiments：
Embodiment 1：
A kind of method for preparing two selenizing rhenium nanometer sheets, comprises the following steps：
Step A：0.5365 gram of ammonium perrhenate, 0.1390 gram of hydroxylamine hydrochloride and 0.6450 gram of selenous acid are dissolved in 60ml water
In, stir 30 minutes, the amount concentration for preparing the total material for obtaining ammonium perrhenate, hydroxylamine hydrochloride and selenous acid is 0.15mol/L's
Homogeneous mixture solotion；
Step B：Mixed solution obtained by step A is shifted in 80ml hydrothermal reaction kettle liners, then by hydro-thermal reaction
Kettle is placed in 240 DEG C of baking ovens and heats, insulation 24 it is small when with maintain chemical reaction progress；After reaction, by hydrothermal reaction kettle
Postcooling is taken out to room temperature, isolated hydrothermal product；
Step C：Hydrothermal product obtained by step B is cleaned with water and alcohol, the drying process under the conditions of 60 DEG C, finally
Two selenizing rhenium nanometer sheets are made.
Fig. 1 is the X-ray diffractogram of two selenizings rhenium nanometer sheet manufactured in the present embodiment, it will be seen from figure 1 that the present embodiment
The product finally synthesized is consistent with the standard PDF cards of two selenizing rheniums, belongs to anorthic system, shows obtained by the embodiment of the present invention
Product is two selenizing rhenium nanometer sheets.
Embodiment 2：
A kind of method for preparing two selenizing rhenium nanometer sheets, comprises the following steps：
Step A：0.5365 gram of ammonium perrhenate, 0.1390 gram of hydroxylamine hydrochloride and 0.4438 gram of selenium dioxide are dissolved in 60ml
In water, stir 30 minutes, the amount concentration for preparing the total material for obtaining ammonium perrhenate, hydroxylamine hydrochloride and selenous acid is 0.10mol/L
Homogeneous mixture solotion；
Step B：Mixed solution obtained by step A is shifted in 80ml hydrothermal reaction kettle liners, then by hydro-thermal reaction
Kettle is placed in 240 DEG C of baking ovens and heats, insulation 24 it is small when with maintain chemical reaction progress；After reaction, by hydrothermal reaction kettle
Postcooling is taken out to room temperature, isolated hydrothermal product；
Step C：Hydrothermal product obtained by step B is cleaned with water and alcohol, the drying process under the conditions of 60 DEG C, finally
Two selenizing rhenium nanometer sheets are made.
Fig. 2 is the Raman spectrogram of two selenizings rhenium nanometer sheet manufactured in the present embodiment, from figure 2 it can be seen that
124cm-1And 174cm-1Occur two Characteristic Raman peaks of two selenizing rheniums at position, show that two selenium are made in the embodiment of the present invention
Change rhenium nanometer sheet.
Embodiment 3：
A kind of method for preparing two selenizing rhenium nanometer sheets, comprises the following steps：
Step A：0.5365 gram of ammonium perrhenate, 0.6949 gram of hydroxylamine hydrochloride and 1.0318 grams of selenous acid are dissolved in 60ml water
In, stir 30 minutes, the amount concentration for preparing the total material for obtaining ammonium perrhenate, hydroxylamine hydrochloride and selenous acid is 0.33mol/L's
Homogeneous mixture solotion；
Step B：Mixed solution obtained by step A is shifted in 80ml hydrothermal reaction kettle liners, then by hydro-thermal reaction
Kettle is placed in 180 DEG C of baking ovens and heats, insulation 24 it is small when with maintain chemical reaction progress；After reaction, by hydrothermal reaction kettle
Postcooling is taken out to room temperature, isolated hydrothermal product；
Step C：Hydrothermal product obtained by step B is cleaned with water and alcohol, the drying process under the conditions of 60 DEG C, finally
Two selenizing rhenium nanometer sheets are made.
Fig. 3 is the x-ray photoelectron spectroscopy figure of two selenizing rheniums prepared by the embodiment of the present invention, be can be seen that from figure (a)：Re
4f valence states correspond respectively to Re 4f at 41.7eV and 44.1eV7/2Track and Re 4f5/2Track, can be seen that from figure (b)：
Se 3d5/2Track and Se 3d3/2Track is 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 for preparing two selenizing rhenium nanometer sheets, comprises the following steps：
Step A：0.5365 gram of ammonium perrhenate, 0.2780 gram of hydroxylamine hydrochloride and 0.6449 gram of selenous acid are dissolved in 60ml water
In, stir 30 minutes, the amount concentration for preparing the total material for obtaining ammonium perrhenate, hydroxylamine hydrochloride and selenous acid is 0.18mol/L's
Homogeneous mixture solotion；
Step B：Mixed solution obtained by step A is shifted in 80ml hydrothermal reaction kettle liners, then by hydro-thermal reaction
Kettle is placed in 260 DEG C of baking ovens and heats, insulation 6 it is small when with maintain chemical reaction progress；After reaction, hydrothermal reaction kettle is taken
Go out postcooling to room temperature, isolated hydrothermal product；
Step C：Hydrothermal product obtained by step B is cleaned with water and alcohol, the drying process under the conditions of 60 DEG C, finally
Two selenizing rhenium nanometer sheets are made.
Fig. 4 is the transmission electron microscope figure of two selenizings rhenium manufactured in the present embodiment, and two selenium are can be clearly seen that 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 for preparing two selenizing rhenium nanometer sheets, comprises the following steps：
Step A：0.5365 gram of ammonium perrhenate, 0.1390 gram of hydroxylamine hydrochloride and 0.8647 gram of sodium selenite are dissolved in 60ml
In water, stir 30 minutes, the amount concentration for preparing the total material for obtaining ammonium perrhenate, hydroxylamine hydrochloride and sodium selenite is 0.15mol/
The homogeneous mixture solotion of L；
Step B：Mixed solution obtained by step A is shifted in 80ml hydrothermal reaction kettle liners, then by hydro-thermal reaction
Kettle is placed in 220 DEG C of baking ovens and heats, insulation 48 it is small when with maintain chemical reaction progress；After reaction, by hydrothermal reaction kettle
Postcooling is taken out to room temperature, isolated hydrothermal product；
Step C：Hydrothermal product obtained by step B is cleaned with water and alcohol, the drying process under the conditions of 60 DEG C, finally
Two selenizing rhenium nanometer sheets are made.
Fig. 5 is the electron scanning micrograph of two selenizings rhenium manufactured in the present embodiment, and two are can be clearly seen that from Fig. 5
The microscopic appearance of selenizing rhenium nanometer sheet.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (3)
- A kind of 1. method for preparing two selenizing rhenium nanometer sheets, it is characterised in that comprise the following steps：Step A：By ammonium perrhenate, hydroxylamine hydrochloride and selenium source according to ammonium perrhenate: hydroxylamine hydrochloride: the amount ratio of the material of selenium source is 10 : 1~60: 20~50 ratio is dissolved in the water, and prepares the amount concentration for the total material for obtaining ammonium perrhenate, hydroxylamine hydrochloride and selenium source For the homogeneous mixture solotion of 0.1~0.4mol/L；Step B：Mixed solution obtained by step A is shifted in hydrothermal reaction kettle, heating hydrothermal reaction kettle is to 180~260 DEG C And keep the temperature to maintain the progress of chemical reaction, after reaction, hydrothermal reaction kettle temperature is cooled to room temperature, isolated hydro-thermal Product；Step C：Hydrothermal product obtained by step B is cleaned with water and alcohol, two selenizing rheniums are finally made after drying process Nanometer sheet.
- 2. a kind of method for preparing two selenizing rhenium nanometer sheets according to claim 1, it is characterised in that in the step B Insulation using maintain chemical reaction time as 6~48 it is small when.
- 3. a kind of method for preparing two selenizing rhenium nanometer sheets according to claim 1, it is characterised in that the selenium source is Asia Selenic acid, selenite or selenium dioxide.
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| 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 |
| CN108862397B (en) * | 2018-06-15 | 2020-08-28 | 肇庆市华师大光电产业研究院 | Method for directly growing uniform rhenium diselenide nanosheet on substrate electrode, modified electrode and application |
| CN111389420B (en) * | 2020-03-25 | 2021-05-28 | 江南大学 | Vacancy-rich rhenium diselenide-based multi-level hydrophobic film and preparation method thereof |
| CN111318288B (en) * | 2020-03-25 | 2021-05-04 | 江南大学 | Rhenium diselenide/carbon nanofiber composite electrocatalytic material 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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| CN105776154A (en) * | 2016-05-10 | 2016-07-20 | 电子科技大学 | Preparation method of tungsten diselenide nanosheet |
| CN105887045A (en) * | 2015-02-16 | 2016-08-24 | 炬力奈米科技有限公司 | Method And Apparatus For Fabricating Two-Dimensional Layered Chalcogenide Film |
| CN105967155A (en) * | 2016-05-10 | 2016-09-28 | 电子科技大学 | Method for preparing tungsten diselenide nanoflower |
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| CN105887045A (en) * | 2015-02-16 | 2016-08-24 | 炬力奈米科技有限公司 | Method And Apparatus For Fabricating Two-Dimensional Layered Chalcogenide Film |
| CN105776154A (en) * | 2016-05-10 | 2016-07-20 | 电子科技大学 | Preparation method of tungsten diselenide nanosheet |
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