CN108217713A - A kind of method that polishing prepares Nano slices of copper sulphide - Google Patents
A kind of method that polishing prepares Nano slices of copper sulphide Download PDFInfo
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- CN108217713A CN108217713A CN201810072442.5A CN201810072442A CN108217713A CN 108217713 A CN108217713 A CN 108217713A CN 201810072442 A CN201810072442 A CN 201810072442A CN 108217713 A CN108217713 A CN 108217713A
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- copper
- copper sulphide
- thiocarbamide
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- mantoquita
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/12—Sulfides
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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 present invention provides a kind of methods that polishing prepares Nano slices of copper sulphide, this method first grinds mantoquita and thiocarbamide in grinding device uniform, it is made to be converted into complex intermediate --- chloride hydrate thiocarbamide closes copper, add in sodium hydroxide thereto again, chloride hydrate thiocarbamide closes and is converted into copper sulfide under oxygen effect of the copper in sodium hydroxide and air.In process of lapping, reaction system in the pasty state, largely limits the diffusion of ion, and so as to slow down nucleation rate, generated copper sulfide nucleus is able to be grown to nanometer sheet.Other reaction products are soluble easily in water or ethyl alcohol, therefore the copper sulfide purity obtained after washing is higher.The Nano slices of copper sulphide of this method preparation is microcosmic to be gone up in uniform laminated structure, nanometer sheet thickness about 12~14nm, which has larger specific surface area and relatively narrow energy gap, is expected to be applied in the fields such as photocatalysis and photocell.This method yield is high, it is easy to accomplish large-scale production.
Description
Technical field
The present invention relates to nano materials to synthesize field, and in particular to a kind of preparation method of nanostructured copper sulfide.
Background technology
In recent years, many researchs find transition metal-chalcogen compound in photocatalysis, electro-catalysis, water process, energy storage
The fields such as device show superior performance.Copper sulfide (CuS), as a kind of important transition metal-chalcogen compound
Semi-conducting material shows unique layer structure, there is the electric conductivity of metalloid and relatively narrow energy gap.Therefore, perhaps
More researchers answering in solar cell, photothermal conversion, photocatalysis, chemical sensor, lithium ion battery electrode material to CuS
It extensive studied with expanding and achieves certain progress.
In order to meet different application demands, zero dimension, one-dimensional, two-dimentional copper sulphide nano structure all there has been successful conjunction
Into strategy.Dong et al. [Ind.Eng.Chem.Res. (2002) 41,4489-4493] and in water/CO2It is made in microemulsion
The CuS nano particles of particle diameter distribution very narrow (2-6nm)；Heydari et al. [Appl.Surf.Sci. (2009) 394,425-430]
Porous CuS hollow nano-spheres are prepared by two step solvent-thermal methods；Hsu et al. [Electrochim.Acta (2014), 139,
401-407] by Cu (OH)2Nano-wire array vulcanization has obtained CuS nano-wire arrays；Mao et al. [Cryst.Growth
Des. (2009), 9,2546-2548] using Cu- thiourea complexs as from sacrifice template CuS porous nanotubes have been made；Peng etc.
People [Mater.Lett. (2014), 122,25-28] and Xu et al. [Electrochim.Acta (2016), 211,891-899] point
CuS nanosheet has not been obtained by the concentrated sulfuric acid removal alloying method of solvent-thermal method and Cu-Ti alloys.It is received in many different CuS
In rice structure, there are the two-dimensional nano piece of nanometer grade thickness and multilevel hierarchy to be studied most, be primarily due to nanometer sheet knot
Structure usually has larger specific surface area and exposed more fully active site, this 2 points for CuS in catalysis and energy storage side
The application in face is highly beneficial.In general, CuS nanosheet is obtained via the removal alloying process of solvent-thermal method or Cu-Ti alloys
's.The former generally requires high temperature and pressure and high viscosity solvent, and the latter is then needed by the use of the sulfuric acid of high concentration as etching agent, and two
Person more takes (a few hours were to 3 days), is unfavorable for large-scale production.Therefore, development is a kind of is simple and efficient, is environmental-friendly
CuS nanosheet synthetic method is most important for the practical application of CuS.
Grinding, as soon as an ancient technology, is applied to early in protohistoric in the processing of cereal.Nowadays, with
The development of mechanical force and chemical, polishing are handed down not only as a kind of method for reducing solid grain size, Er Qiecheng
In order to which a kind of green, economic solid material synthesis strategy are further developed.Polishing is without solvent, without additional
Heat and pressure can quickly realize being prepared on a large scale for product under the auxiliary of ball mill.Li et al. people [Appl.Surf.Sci.
(2016), 384,272-278] by ball mill directly by sulphur powder and copper powder through a step mechanical milling process be made grain size 5nm with
Under CuS quantum dots, and the method be expected to realize large-scale production.This inspires us to be expected to be used for CuS nanosheet by polishing
In preparation.
Invention content
The object of the present invention is to provide a kind of methods that polishing prepares Nano slices of copper sulphide, and this method yield is high, is easy to
It accomplishes scale production.
Nano slices of copper sulphide prepared by the present invention, chemical formula are CuS or (Cu+)3(S2-)(S2 -), in uniform sheet
Structure.
Preparation method provided by the invention is first to grind mantoquita and thiocarbamide uniformly in grinding device, is converted into it
Chloride hydrate thiocarbamide closes copper (I) intermediate, then adds in sodium hydroxide thereto, oxygen of the intermediate in sodium hydroxide and air
Under the action of be converted into copper sulfide.
The preparation method of Nano slices of copper sulphide of the present invention, concrete operations are as described below：
A. mantoquita and thiocarbamide are added in grinding device, the molar ratio of wherein mantoquita and thiocarbamide is 1:2-6, grinding is until obtain
To uniform green mixture.
The mantoquita is anhydrous CuCl2Or CuCl2·2H2O, the grinding device is mortar, planetary ball mill, pipe
Formula ball mill or pyramid type ball mill.
B. NaOH is added in the mixture of step A, the molar ratio of wherein NaOH and mantoquita is 1-6:1, continue to grind
Mill until mixture in black paste, by pasty mixture deionized water and absolute ethyl alcohol centrifuge washing 3-6 times, to wash away pair
Product bis-thiourea and NaCl and unreacted thiocarbamide that may be present and NaOH in 60 DEG C of drying, obtain the copper sulfide of high-purity
Nanometer sheet.
The present invention can be realized the preparation of Nano slices of copper sulphide in the unlimited system for being exposed to air, in process of lapping,
Reaction system in the pasty state, largely limits the diffusion of ion, and so as to slow down nucleation rate, the copper sulfide for making generation is brilliant
Nucleus growth is nanometer sheet.Other reaction products are soluble easily in water or ethyl alcohol, therefore the copper sulfide purity obtained after washing is higher.
Any solvent is not needed in entire process of lapping, it is not required that heating,
Pattern and performance characterization are carried out to sample obtained above
Fig. 1 is scanning electron microscope (SEM) characterization for the Nano slices of copper sulphide that 1 step B of embodiment is obtained, can by figure
See, in the form of sheets, surface is relatively smooth for the microstructure of product, thickness about 12nm, and border width is differed for tens to hundreds of nanometers.
Fig. 2 is scanning electron microscope (SEM) characterization for the Nano slices of copper sulphide that 4 step B of embodiment is obtained, can by figure
See, in the form of sheets, surface is relatively smooth for the microstructure of product, thickness about 14nm, and border width is differed for tens to hundreds of nanometers.
Illustrate that magnanimity preparation still can obtain flaky nanometer structure, also illustrate that this method is expected to realize the scale metaplasia of Nano slices of copper sulphide
Production.
The X-ray diffraction (XRD) of the Nano slices of copper sulphide characterization that Fig. 3 is embodiment 1 and 4 step B of embodiment is obtained, spreads out
Peak is penetrated to comply fully with, and without apparent impurity diffraction maximum, say with copper sulfide standard x RD cards (JCPDS Card 06-0464)
The Nano slices of copper sulphide of bright gained has higher purity, while also illustrates that magnanimity preparation can also obtain the vulcanization of higher degree
Copper nanometer sheet.
The Raman Characterization of Nano slices of copper sulphide that Fig. 4 is embodiment 1 and 4 step B of embodiment is obtained is being drawn in spectrogram
Graceful displacement is 137.3cm-1、261.9cm-1、471.0cm-1Position there is the characteristic peak of copper sulfide, and without apparent miscellaneous
Mass peak further illustrates the Nano slices of copper sulphide for illustrating that polishing can obtain very high-purity.
Fig. 5 is the nitrogen Adsorption and desorption isotherms characterization for the Nano slices of copper sulphide that 1 step B of embodiment is obtained and BET equations point
(as is shown in said inset), as seen from the figure, the nitrogen adsorption isotherm for the Nano slices of copper sulphide that embodiment 1 obtains shows II type etc. for analysis
The feature of warm line, and there are H3 type hysteresis loops in desorption isotherm, shows that duct is wedged hole in sample, is further illustrated real
The copper sulfide for applying 1 gained of example is laminated structure.BET is analysis shows the specific surface area of Nano slices of copper sulphide is obtained by embodiment
23.18m2·g-1。
Fig. 6 is the nitrogen Adsorption and desorption isotherms characterization for the Nano slices of copper sulphide that 4 step B of embodiment is obtained and BET equations point
(as is shown in said inset), as seen from the figure, the nitrogen adsorption isotherm for the Nano slices of copper sulphide that embodiment 4 obtains shows II type etc. for analysis
The feature of warm line, and there are H3 type hysteresis loops in desorption isotherm, shows that wherein duct is wedged hole, further illustrates and implements
The copper sulfide of 4 gained of example is laminated structure.But with Fig. 5 comparisons as it can be seen that when relative pressure is identical, 4 gained copper sulfide nano of embodiment
The adsorbance of rice piece is smaller than the Nano slices of copper sulphide of 1 gained of embodiment, and BET analyses also indicate that 4 gained copper sulphide nano of embodiment
The specific surface area of piece is 11.04m2·g-1, this may be to need the longer reaction time because prepared by magnanimity, and the reaction time
Extend the reunion for resulting in nanometer sheet to a certain extent.
Fig. 7 is the UV-Vis DRS spectrum (UV-Vis DRS) for the Nano slices of copper sulphide that 1 step B of embodiment is obtained
Characterization and Tauc plot analysis results (as is shown in said inset), by spectrogram as it can be seen that the Nano slices of copper sulphide of the gained of embodiment 1 is can
See-there is wider absorption peak in near-infrared region, Tauc plot are analysis shows its energy gap is 1.81eV.
Fig. 8 is the UV-Vis DRS spectrum (UV-Vis DRS) for the Nano slices of copper sulphide that 4 step B of embodiment is obtained
Characterization and Tauc plot analysis results (as is shown in said inset), by spectrogram as it can be seen that the Nano slices of copper sulphide of the gained of embodiment 1 is can
See-there is wider absorption peak in near-infrared region, Tauc plot are analysis shows its energy gap is 1.83eV.Fig. 7's and Fig. 8
Characterization illustrates that Nano slices of copper sulphide obtained by polishing has relatively narrow energy gap, there is potential answer in fields such as photocatalysis, photocells
Use prospect.
Beneficial effects of the present invention：The polishing can be realized in the unlimited system for being exposed to air, and the sulphur of output
It is higher to change copper nanometer sheet purity.In addition to product copper sulfide, other reaction products are soluble easily in water or ethyl alcohol, therefore pass through washing
It can obtain the copper sulfide of higher degree.The product Nano slices of copper sulphide of preparation has larger specific surface area and relatively narrow energy gap,
There is wider absorption peak in visible-near-infrared area, have potential application prospect in fields such as photocell, photocatalysis.It should
Preparation method is not needed to using organic solvent, it is not required that heating, therefore with it is easy, efficient, environmentally friendly, at low cost, be easy to criticize
Amount production.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) characterization of the Nano slices of copper sulphide in embodiment 1.
Fig. 2 is scanning electron microscope (SEM) characterization of the Nano slices of copper sulphide of 4 step B of embodiment.
Fig. 3 is X-ray diffraction (XRD) characterization of the Nano slices of copper sulphide of embodiment 1 and embodiment 4.
Fig. 4 is the Raman Characterization of the Nano slices of copper sulphide of embodiment 1 and embodiment 4.
Fig. 5 is the nitrogen Adsorption and desorption isotherms characterization of the Nano slices of copper sulphide in embodiment 1 and BET equation analysis.
Fig. 6 is the nitrogen Adsorption and desorption isotherms characterization of the Nano slices of copper sulphide in embodiment 4 and BET equation analysis.
Fig. 7 be the Nano slices of copper sulphide in embodiment 1 UV-Vis DRS spectrum (UV-Vis DRS) characterization and
Tauc plot analysis results.
Fig. 8 be the Nano slices of copper sulphide in embodiment 4 UV-Vis DRS spectrum (UV-Vis DRS) characterization and
Tauc plot analysis results.
Specific embodiment
Embodiment 1
A. agate mortar and agate pestle are cleaned and is dried with deionized water and absolute ethyl alcohol.Weigh 0.34g CuCl2·
2H2O and 0.31g thiocarbamides are placed in agate mortar, are ground 5min with agate pestle, are obtained jade-green mixture.
B. 0.20g sodium hydroxides are weighed to be placed in the mixture obtained by step A, continues grinding 5min and obtains black paste
Mixture.After paste is collected and distinguishes centrifuge washing for several times with deionized water and absolute ethyl alcohol, in 60 DEG C of drying, obtain
To dirty-green powder be Nano slices of copper sulphide.Obtained Nano slices of copper sulphide is weighed, result 0.189g, according to
CuCl2·2H2The dosage of O calculates theoretical yield as 0.191g, therefore yield is 99.0%.To obtained Nano slices of copper sulphide
Nitrogen Adsorption and desorption isotherms test is carried out, as a result sees Fig. 5, calculating it according to BET method goes out specific surface area for 23.18m2·g-1.It is right
Obtained Nano slices of copper sulphide carries out UV-Vis DRS test, as a result sees Fig. 7, its taboo is calculated according to Tauc plot methods
Bandwidth is 1.81eV.
Embodiment 2
A. agate mortar and agate pestle are cleaned and is dried with deionized water and absolute ethyl alcohol.Weigh the anhydrous CuCl of 0.27g2
It is placed in agate mortar with 0.31g thiocarbamides, 5min is ground with agate pestle, obtains the mixture of white.
B. 0.20g sodium hydroxides are weighed to be placed in the mixture obtained by step B, continues grinding 5min and obtains black paste
Mixture.After paste is collected and distinguishes centrifuge washing for several times with deionized water and absolute ethyl alcohol, in 60 DEG C of drying, obtain
To dirty-green powder be Nano slices of copper sulphide.Obtained Nano slices of copper sulphide is weighed, result 0.188g, according to anhydrous
CuCl2Dosage calculate theoretical yield as 0.191g, therefore yield is 98.4%.
Embodiment 3
A. polytetrafluoroethylene (PTFE) ball grinder and zirconium oxide abrasive ball are cleaned and is dried with deionized water and absolute ethyl alcohol.It weighs
20.5g CuCl2·2H2O and 31.3g thiocarbamides are placed in ball grinder, are added in appropriate zirconium oxide abrasive ball, are put into planetary ball mill
Middle grinding 10min grinds reactant uniform.
B. it weighs 16.5g sodium hydroxides to be placed in the mixture obtained by step A, since reaction will release a large amount of gases, first
With clean and dry glass bar by mixture stir about 2min in ball grinder, until it is no longer released gas and in black, then will
Ball grinder seal and be put into continue in planetary ball mill grind 20min obtain the mixture of black paste.Paste is subject to
After collecting and distinguishing centrifuge washing for several times with deionized water and absolute ethyl alcohol, in 60 DEG C of drying, obtained dirty-green powder is
Nano slices of copper sulphide.Obtained Nano slices of copper sulphide is weighed, result 11.1g, according to CuCl2·2H2The dosage of O calculates
Theoretical yield is 11.5g, therefore yield is 96.5%.
Embodiment 4
The embodiment is the amplification test according to the ratio progress of embodiment 1
A. polytetrafluoroethylene (PTFE) ball grinder and zirconium oxide abrasive ball are cleaned and is dried with deionized water and absolute ethyl alcohol.It weighs
20.5gCuCl2·2H2O and 20.0g thiocarbamides are placed in ball grinder, are added in appropriate zirconium oxide abrasive ball, are put into planetary ball mill
Middle grinding 10min grinds reactant uniform.
B. it weighs 10.5g sodium hydroxides to be placed in the mixture obtained by step A, since reaction will release a large amount of gases, first
With clean and dry glass bar by mixture stir about 2min in ball grinder, until it is no longer released gas and in black, then will
Ball grinder seal and be put into continue in planetary ball mill grind 20min obtain the mixture of black paste.Paste is subject to
After collecting and distinguishing centrifuge washing for several times with deionized water and absolute ethyl alcohol, in 60 DEG C of drying, obtained dirty-green powder is
Nano slices of copper sulphide, yield reach 97.8%.Obtained Nano slices of copper sulphide is weighed, result 11.3g, according to CuCl2·
2H2The dosage of O calculates theoretical yield as 11.5g, therefore yield is 98.3%.It is obtained by Fig. 6 and 8, specific surface area is it
11.04m2·g-1, energy gap 1.83eV.
Claims (2)
1. a kind of method that polishing prepares Nano slices of copper sulphide, is as follows：
A. mantoquita and thiocarbamide are added in grinding device, the molar ratio of wherein mantoquita and thiocarbamide is 1:2-6, grinding is until obtain
One green mixture, chloride hydrate thiocarbamide close copper；The mantoquita is anhydrous CuCl2Or CuCl2·2H2O；
B. NaOH is added in the mixture of step A, the molar ratio of wherein NaOH and mantoquita is 1-6:1, continue grinding until mixed
Object is closed in black paste, by pasty mixture deionized water and absolute ethyl alcohol centrifuge washing 3-6 time, to wash away by-product pair sulphur
Urea, NaCl and unreacted thiocarbamide and NaOH in 60 DEG C of drying, obtain Nano slices of copper sulphide, and chemical formula is CuS or (Cu+)3
(S2-)(S2 -), microscopic appearance is in uniform laminated structure, and nanometer sheet thickness is 12~14nm.
2. the method that polishing according to claim 1 prepares Nano slices of copper sulphide, it is characterized in that the grinding device
For planetary ball mill or tube mill.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1958459A (en) * | 2006-11-23 | 2007-05-09 | 上海交通大学 | Method for preparing hexagonal Nano slices of copper sulphide |
| CN102320647A (en) * | 2011-08-17 | 2012-01-18 | 北京科技大学 | Preparation method of copper sulphide nano-powder with different stoichiometric ratios |
| CN107352574A (en) * | 2017-08-24 | 2017-11-17 | 北京化工大学 | A kind of preparation method of three-dimensional structure nano-copper sulfide |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1958459A (en) * | 2006-11-23 | 2007-05-09 | 上海交通大学 | Method for preparing hexagonal Nano slices of copper sulphide |
| CN102320647A (en) * | 2011-08-17 | 2012-01-18 | 北京科技大学 | Preparation method of copper sulphide nano-powder with different stoichiometric ratios |
| CN107352574A (en) * | 2017-08-24 | 2017-11-17 | 北京化工大学 | A kind of preparation method of three-dimensional structure nano-copper sulfide |
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