CN105668526B - A kind of preparation method of nanoporous tellurium - Google Patents
A kind of preparation method of nanoporous tellurium Download PDFInfo
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- CN105668526B CN105668526B CN201610170586.5A CN201610170586A CN105668526B CN 105668526 B CN105668526 B CN 105668526B CN 201610170586 A CN201610170586 A CN 201610170586A CN 105668526 B CN105668526 B CN 105668526B
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- tellurium
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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
- C01B19/02—Elemental selenium or tellurium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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Abstract
The present invention relates to a kind of preparation method of nanoporous tellurium, belong to nano material, the preparing technical field of porous material.The preparation method refers to pore creating material and the grinding of tellurium powder uniformly obtaining mixture, static state heating mixture melts to whole, room temperature is naturally cooled to again to obtain solidifying presoma, solidification presoma is inserted in the solvent that can dissolve pore creating material, make pore creating material dissolving complete, undissolved solid is taken out, is cleaned and dried using deionized water, produces nanoporous tellurium material.Nano-pore is prepared using the method for dissolving pore creating material, by controlling the mass ratio of pore creating material and tellurium, prepares the nanoporous tellurium of different pore size.Preparation method design is unique, and aggregate velocity is fast, and heating-up temperature is low, and the time is short, can solve because heating-up temperature is high in conventional preparation techniques, and the time is long and can not form the problem of nano-pore is with nano-structure is retained.Simple to operate, easy popularization and application of the invention.
Description
Technical field
The present invention relates to a kind of preparation method of nanoporous tellurium, belong to nano material, porous material preparing technical field.
Background technology
Tellurium, it is a kind of narrow-band semiconductor material, there is excellent optics, photoelectricity and thermoelectricity capability, is to make semiconductor, system
The ideal material of cold element, photoelectric cell etc., it is described as " vitamin of modern industry, national defence and sophisticated technology, it is strange creating the human world
The bridge of mark ", " being the backing material of contemporary high-tech art new material ".Simultaneously as its unique anisotropic growth tendency
With potential application, the nanostructured for synthesizing tellurium causes scientific circles and more and more paid attention to.At present, there are some researches show nano junction
The tellurium of structure, tellurium can be assigned in the more unique advantages in the fields such as light guide, thermoelectricity, photoelectricity, piezoelectricity and nonlinear optical sensing.Such as exist
Entitled " Formation of single- disclosed in document J. Mater. the 20th phases of Chem. page 2457-2463 of 2010
crystal tellurium nanowires and nanotubes via hydrothermal recrystallization
The controllable hydro-thermal legal system of size is taken in and their gas sensing properties at room temperature "
Ammonia air pressure inductor can be used at ambient temperature by obtaining the tellurium nano-wire of size uniformity.And for example in the document J. of 2011
Chin. entitled " Selective Tellurium Nanowire- disclosed in 732-738 pages of the phases of Chem. Soc. the 58th
The method system that tellurium oxide is reduced is taken in based Sensors for Mercury (II) in Aqueous Solution "
The tellurium nano-wire obtained is used for the induction monitoring of dimercurion in aqueous phase.In addition, the tellurium of nanostructured is alternatively arranged as template
For preparing monodimension nanometer material, as disclosed in document J. Phys. Chem. the 20th phases of C page 1727-1737 of 2009
Entitled " Tellurium nanowire-induced room temperature conversion of graphite
Tellurium nano-wire can promote graphene oxide to be changed into lobate in oxide to leaf-like graphenic structures "
The graphene of structure.Three-D nano-porous material, not only with special porous microscopic appearance, is gone back due to the introducing of loose structure
Have the characteristics that specific surface area is high, pore passage structure is abundant, aperture is adjustable, in catalysis, absorption, ion exchange and electrochemical energy storage etc.
Aspect, which is obtained for, to be widely applied.Therefore, the preparation nanoporous tellurium material that specific surface area is big, porosity is high is to promoting tellurium
Had important practical significance using with development.But the tellurium that three-D nano-porous structure is prepared for mass is not yet reported that.
The content of the invention
It is an object of the invention to provide a kind of preparation method of nanoporous tellurium.
To achieve these goals, the present invention uses following technical scheme：
A kind of preparation method of nanoporous tellurium, the preparation method refer to uniformly be mixed pore creating material and the grinding of tellurium powder
Zoarium, static state heating mixture is to all meltings, then naturally cools to room temperature and obtain solidifying presoma, and solidification presoma is inserted
In the solvent that pore creating material can be dissolved, make pore creating material dissolving complete, take out undissolved solid, cleaned and done using deionized water
It is dry, nanoporous tellurium material is produced, preparation method is carried out according to the following steps：
A inserts pore creating material in the mortar for filling tellurium powder, grinds 30 ~ 60 minutes, to ensure that pore creating material and tellurium powder are fully mixed
Close, obtain mixture, wherein pore creating material and tellurium powder mass ratio are 0.1 ~ 10；
The mixture static state of pore creating material in step a and tellurium powder is heated to stop heating after all meltings by b, natural cooling
To room temperature, obtain solidifying presoma；
C, which inserts the solidification presoma in step b in the solvent of dissolving pore creating material, to be soaked, after pore creating material dissolving completely,
Undissolved solid is taken out, deionized water cleaning is reused, the nanoporous tellurium material is produced after being dried under 60 ~ 90 oC.
The pore creating material is one kind in sulphur powder or selenium powder.
The solvent of the dissolving pore creating material is one kind in carbon disulfide or benzene or carbon tetrachloride or dichloromethane.
The nanoporous tellurium material aperture is 10 ~ 100nm.
As a result of above technical scheme, the preparation method of nanoporous tellurium material of the invention, using low melting point
Tellurium powder is matrix host material, and the method using grinding stirring is sufficiently mixed pore creating material and tellurium powder, then static heating makes pore-creating
Agent melts jointly with tellurium powder, pore creating material is fully dissolved and is stayed in material of main part matrix using pore creating material solvent after cooling
Under it is nano level porous, nanoporous tellurium material is prepared.Nano-pore is prepared using the method for dissolving pore creating material, passes through change
The mass ratio of pore creating material and tellurium, the nanoporous tellurium of different pore size can be prepared.Tellurium reaches Nano grade, its light guide, thermoelectricity, light
The performances such as electricity, piezoelectricity and nonlinear optical sensing are obtained for raising.Nanoporous tellurium prepared by the present invention compared with 1-dimention nano tellurium,
Possess bigger specific surface area and abundant pore passage structure, for being catalyzed, adsorbing, ion exchange and electrochemical energy storage etc. energy
Enough show more excellent performance.Preparation method design is unique, aggregate velocity is fast, heating-up temperature is low, the time is short, can solve
Because heating-up temperature is high in conventional preparation techniques (such as " high-temperature sintering process "), the time is long and can not form nano-pore and retain nanometer
It is the problem of tissue, simple to operate, thus the present invention method after popularization and application, will produce huge social benefit and
Economic benefit.
Embodiment
With reference to embodiment, the invention will be further elaborated.
A kind of preparation method of nanoporous tellurium, the preparation method refer to uniformly be mixed pore creating material and the grinding of tellurium powder
Zoarium, static state heating mixture is to all meltings, then naturally cools to room temperature and obtain solidifying presoma, and solidification presoma is inserted
In the solvent that pore creating material can be dissolved, make pore creating material dissolving complete, take out undissolved solid, cleaned and done using deionized water
It is dry, nanoporous tellurium material is produced, preparation method is carried out according to the following steps：
A inserts pore creating material in the mortar for filling tellurium powder, grinds 30 ~ 60 minutes, to ensure that pore creating material and tellurium powder are fully mixed
Close, obtain mixture, wherein pore creating material and tellurium powder mass ratio are 0.1 ~ 10；
The mixture static state of pore creating material in step a and tellurium powder is heated to stop heating after all meltings by b, natural cooling
To room temperature, obtain solidifying presoma；
C, which inserts the solidification presoma in step b in the solvent of dissolving pore creating material, to be soaked, after pore creating material dissolving completely,
Undissolved solid is taken out, deionized water cleaning is reused, the nanoporous tellurium material is produced after being dried under 60 ~ 90 oC.
The pore creating material is one kind in sulphur powder or selenium powder.
The solvent of the dissolving pore creating material is one kind in carbon disulfide or benzene or carbon tetrachloride or dichloromethane.
The nanoporous tellurium material aperture is 10 ~ 100nm.
Embodiment 1
A inserts 1g sulphur powders in the mortar for filling 10g tellurium powder, grinds 30 minutes, to ensure that sulphur powder and tellurium powder are fully mixed
Close, obtain mixture；
The mixture static state of sulphur powder in step a and tellurium powder is heated to stop heating after all meltings by b, is naturally cooled to
Room temperature, obtain solidifying presoma；
C, which inserts the solidification presoma in step b in carbon disulfide solvent, to be soaked, and after sulphur powder dissolving completely, is taken out not
The solid of dissolving, deionized water cleaning is reused, the nanoporous tellurium material that aperture is 10nm is produced after being dried under 60 oC.
Embodiment 2
A inserts 15g selenium powders in the mortar for filling 3g tellurium powder, grinds 50 minutes, to ensure that selenium powder and tellurium powder are fully mixed
Close, obtain mixture；
The mixture static state of selenium powder in step a and tellurium powder is heated to stop heating after all meltings by b, is naturally cooled to
Room temperature, obtain solidifying presoma；
C, which inserts the solidification presoma in step b in carbon tetrachloride solvent, to be soaked, and after selenium powder dissolving completely, is taken out not
The solid of dissolving, deionized water cleaning is reused, the nanoporous tellurium material that aperture is 50nm is produced after being dried under 75 oC.
Embodiment 3
A inserts 40g sulphur powders in the mortar for filling 4g tellurium powder, grinds 60 minutes, to ensure that sulphur powder and tellurium powder are fully mixed
Close, obtain mixture；
The mixture static state of sulphur powder in step a and tellurium powder is heated to stop heating after all meltings by b, is naturally cooled to
Room temperature, obtain solidifying presoma；
C, which inserts the solidification presoma in step b in dichloromethane solvent, to be soaked, and after sulphur powder dissolving completely, is taken out not
The solid of dissolving, deionized water cleaning is reused, the nanoporous tellurium material that aperture is 100nm is produced after being dried under 90 oC.
Embodiment 4
A inserts 40g sulphur powders in the mortar for filling 4g tellurium powder, grinds 60 minutes, to ensure that sulphur powder and tellurium powder are fully mixed
Close, obtain mixture；
The mixture static state of sulphur powder in step a and tellurium powder is heated to stop heating after all meltings by b, is naturally cooled to
Room temperature, obtain solidifying presoma；
C, which inserts the solidification presoma in step b in benzene solvent, to be soaked, and after sulphur powder dissolving completely, is taken out undissolved
Solid, deionized water cleaning is reused, the nanoporous tellurium material that aperture is 100nm is produced after being dried under 90 oC.
Claims (3)
- A kind of 1. preparation method of nanoporous tellurium, it is characterised in that：The preparation method refers to pore creating material sulphur powder or selenium powder Uniformly mixture is obtained with the grinding of tellurium powder, and static state heating mixture is to all meltings, then naturally cools to before room temperature obtains solidification Body is driven, solidification presoma is inserted in the solvent that can dissolve pore creating material, makes pore creating material dissolving complete, takes out undissolved solid, Cleaned and dried using deionized water, produce nanoporous tellurium material, preparation method is carried out according to the following steps：A inserts pore creating material in the mortar for filling tellurium powder, grinds 30 ~ 60 minutes, to ensure that pore creating material and tellurium powder are sufficiently mixed, Mixture is obtained, wherein pore creating material and tellurium powder mass ratio are 0.1 ~ 10；The mixture static state of pore creating material in step a and tellurium powder is heated to stop heating after all meltings by b, naturally cools to room Temperature, obtain solidifying presoma；C, which inserts the solidification presoma in step b in the solvent of dissolving pore creating material, to be soaked, and after pore creating material dissolving completely, is taken out Undissolved solid, deionized water cleaning is reused, the nanoporous tellurium material is produced after being dried under 60 ~ 90 oC.
- 2. the preparation method of a kind of nanoporous tellurium according to claim 1, it is characterised in that the dissolving pore creating material Solvent is one kind in carbon disulfide or benzene or carbon tetrachloride or dichloromethane.
- A kind of 3. preparation method of nanoporous tellurium according to claim 1, it is characterised in that the nanoporous tellurium material Blanking aperture is 10 ~ 100nm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU410796A1 (en) * | 1972-02-15 | 1974-01-15 | ||
| CN101656292A (en) * | 2009-09-16 | 2010-02-24 | 北京科技大学 | Preparation method for bismuth-tellurium nano-porous thermoelectric material |
| CN102351168A (en) * | 2011-07-07 | 2012-02-15 | 浙江大学 | Preparation method of vinylidene chloride polymer base mesopore-micropore composite porous charcoal |
| CN103628106A (en) * | 2013-11-01 | 2014-03-12 | 大连理工大学 | Method for preparing indium/tellurium porous nanowire array |
-
2016
- 2016-03-24 CN CN201610170586.5A patent/CN105668526B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU410796A1 (en) * | 1972-02-15 | 1974-01-15 | ||
| CN101656292A (en) * | 2009-09-16 | 2010-02-24 | 北京科技大学 | Preparation method for bismuth-tellurium nano-porous thermoelectric material |
| CN102351168A (en) * | 2011-07-07 | 2012-02-15 | 浙江大学 | Preparation method of vinylidene chloride polymer base mesopore-micropore composite porous charcoal |
| CN103628106A (en) * | 2013-11-01 | 2014-03-12 | 大连理工大学 | Method for preparing indium/tellurium porous nanowire array |
Non-Patent Citations (1)
| Title |
|---|
| Nanoporous selenium as acathode material for rechargeable lithium–selenium batteries;Lili Liu et al.;;《ChemComm》;20131009;第49卷;第111515－11517页 * |
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