CN108441652A - A kind of preparation method of mesoporous germanium material - Google Patents
A kind of preparation method of mesoporous germanium material Download PDFInfo
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- CN108441652A CN108441652A CN201810218031.2A CN201810218031A CN108441652A CN 108441652 A CN108441652 A CN 108441652A CN 201810218031 A CN201810218031 A CN 201810218031A CN 108441652 A CN108441652 A CN 108441652A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B41/00—Obtaining germanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The present invention relates to a kind of preparation methods of mesoporous germanium material, belong to the technical field of preparation and the application of germanium material, it is using germanium tetrachloride as ge source, using Na-K alloy as reducing agent, using toluene as solvent, through magnetic agitation at room temperature, reaction solution is made, through filtering, roasting, washing, vacuum drying, mesoporous germanium material is made, this preparation method technique is advanced, informative data is accurate, it is fast to prepare speed, product is black powder, with mesopore orbit structure, products collection efficiency is high, up to 95.2%, it can be used as lithium ion battery negative material, it is the very ideal method for preparing mesoporous germanium material.
Description
Technical field
The present invention relates to a kind of preparation methods of mesoporous germanium material, belong to the technical field of preparation and the application of germanium material.
Background technology
Mesoporous germanium material has good adjustability of structure and electro-chemical activity, is that other materials is incomparable, mesoporous
Germanium material has higher specific surface area and larger pore volume, is widely applied in absorption, catalysis, electricity field.
The synthetic method and process of mesoporous germanium material will have a direct impact on the structure feature and performance of material, synthetic method and mould
The selection of plate agent is conclusive influence factor, and reaction temperature, reaction time and calcination temperature are also to the duct of porous germanium material
Structure has important influence.
Template is the element for preparing mesoporous germanium material, and presoma passes through supermolecule power or change with template
Act on forming into meso-hole structure.The structure and type of template will influence the pore passage structure of mesoporous germanium material, therefore template
Selection and use be highly important.
During using germanium tetrachloride as the mesoporous germanium material of precursor synthesis, it is required for using soft template or hard template greatly
As structure directing agent, since the chemical substance of selection is different, the difference of synthetic parameters, the difference of building-up process, calcination temperature
From 600 DEG C to 1000 DEG C, the mesoporous germanium material Chemical Physics performance difference of gained is larger, it is difficult to meet the requirement of synthetic, makes
The application of such material receives significant limitation.
Invention content
The purpose of the present invention is in view of the above-mentioned problems, using a kind of new metal reduction synthesis process, make gold with Na-K alloy
Belong to reducing agent to stir at ambient temperature using germanium tetrachloride as presoma, the black powder of gained passes through tube furnace high-temperature roasting
Mesoporous germanium material is prepared, can reach adjusting germanium material pore passage structure by controlling calcination temperature, improve Chemical Physics performance, it should
Material can be used as lithium ion battery negative material.
Technical scheme is as follows：A kind of preparation method of mesoporous germanium material, the chemicals material that this method includes
Material is：Metallic sodium, metallic potassium, germanium tetrachloride, toluene, ethyl alcohol, deionized water；
A combination thereof dosage is as follows：It is measurement unit with gram, milliliter,
Preparation method includes the following steps：
(1) Na-K alloy is prepared：Metallic sodium 0.4g ± 0.03g is weighed, metallic potassium 1.6g ± 0.04g is weighed, stirs 1min,
It is configured to Na-K alloy；
(2) synthesising mesoporous germanium material：Under nitrogen protection, reduction is first stirred at room temperature, solid is obtained by filtration later, most
High-temperature roasting under a nitrogen atmosphere afterwards, obtains product of roasting；
(3) it washs, filter：
(4) it is dried in vacuo：It is mesoporous germanium material after drying；
(5) test, analysis and characterization：The pattern, ingredient, Chemical Physics performance of the mesoporous germanium body material of preparation are examined
It surveys, analysis, characterize.
Step (2) specifically includes as follows：
A, hybrid reaction mixture is prepared：2.4 ± 0.04g of germanium tetrachloride, 1.8 ± 0.03g of Na-K alloy are weighed, first is measured
Benzene 200mL ± 5mL is added in round-bottomed flask, at mixed reaction solution；
B, magnetic agitation, mixing time 4h are opened, mixed reaction solution is reacted, and reaction equation is as follows：
GeCl4+ 4Na=4NaCl+Ge
GeCl4+ 4K=4KCl+Ge
C, after the completion of reaction, stop stirring, ethyl alcohol 100ml is added；It filters：Mixture after reaction is placed in bottle,suction
It in Buchner funnel, is filtered with miillpore filter, remaining product filter cake waste liquid is evacuated in filter flask on filter membrane；Roasting：By gained
For filter cake in tubular type kiln roasting, temperature is 300-600 DEG C.
The step (3) washing, filter the specific steps are：Product of roasting is placed in beaker, deionized water is added
100mL, agitator treating 5min；Cleaning solution is placed in the Buchner funnel of bottle,suction, is filtered with miillpore filter, is stayed on filter membrane
Product cake is deposited, cleaning solution is evacuated in filter flask, and washing filters progress 2 times；Product cake is placed in beaker, deionization is added
Water 100mL, agitator treating 5min, washing filter progress 2 times.
The step (4) it is vacuum drying the specific steps are：Product cake after washing is placed in quartz container, then
It is placed in vacuum drying chamber and is dried, 50 DEG C ± 1 DEG C of drying temperature, vacuum degree 50Pa, drying time 10h.
The mesoporous germanium material can be applied to lithium ion battery negative material.
Beneficial effects of the present invention：The present invention has apparent advanced compared with prior art, be germanium tetrachloride is germanium
Using Na-K alloy as reducing agent, using toluene as solvent, through magnetic agitation at room temperature, reaction solution is made in source, through suction filtration, height
Temperature roasting, washing, vacuum drying, are made mesoporous germanium material, this preparation method technique is advanced, and informative data is accurate, prepare speed
Soon, it is not necessarily to additional template, product is black powder, has mesopore orbit structure, products collection efficiency is high, up to 95.2%, can make
It is the very ideal method for preparing mesoporous germanium material for lithium ion battery negative material.
Description of the drawings
The present invention will be further described below with reference to the drawings.
It is above-mentioned purpose of the invention, excellent by reference to the detailed description below in conjunction with attached drawing to used embodiment
Point and feature will become more apparent from, wherein：
Fig. 1 is that mesoporous germanium material is synthetically prepared required glass round bottom flask structural schematic diagram；
1, iron clamp, 2, round-bottomed flask, 3, mixing platform, 4, fixed link, 5, magnetic stir bar, 6, plastics rubber plug, 7, blender
Seat, 8, display screen, 9 indicator lights, 10 power switches, 11 rotation speed regulating and controlling devices.
Fig. 2 is that mesoporous germanium material is synthetically prepared required tube furnace structural schematic diagram；
1 air inlet, 2 vacuum orifices, 3 flanges, 4 protective covers, 5 knobs, 6 voltages, ammeter, 7 control buttons, 8 pulling buckles lock,
9 temperature controllers, 10 pressure gauges, 11 gas outlets；
Fig. 3 is the X ray diffracting spectrum of mesoporous germanium material；
Fig. 4 is mesoporous germanium material nitrogen adsorption desorption curve figure；
Fig. 5 is mesoporous germanium material transmission electron microscope photo；
Fig. 6 show cycle performance curve graph of the mesoporous germanium material as lithium ion battery negative material.
Specific implementation mode
Carry out detailed description of the present invention specific implementation mode below with reference to the accompanying drawings.
Shown in Fig. 1 and Fig. 2, it is synthetically prepared state diagram for mesoporous germanium material, as shown in the figure, each portion position is correct, according to quantity
Proportioning, sequentially operates；The magnitude for preparing the chemical substance used is determined by pre-set range, by gram, milliliter in terms of
Measure unit.
The synthesis of mesoporous germanium material is carried out in glass round bottom flask and tube furnace, is by process and inertia is stirred at room temperature
High-temperature roasting is completed under atmosphere；
Such as Fig. 1, blender is rectangle, round-bottomed flask 2 is fixed in the fixed link 4 of mixing platform 3 using iron clamp 1, magnetic force
Stirrer 5 is placed in drag, and round-bottomed flask bottleneck is sealed with plastics rubber plug 6.Display screen 8, instruction are equipped on blender base 7
Lamp 9, power switch 10, rotation speed regulating and controlling device 11.
Such as Fig. 2, high-temperature roasting carries out in tubular type, and with nitrogen as protection gas, calcination temperature is 300-600 DEG C.1
Air inlet, 2 vacuum orifices, 3 flanges, 4 protective covers, 5 knobs, 6 voltages, ammeter, 7 control buttons, 8 pulling buckles lock, 9 temperature controllers,
10 pressure gauges, 11 gas outlets；
The chemical substance material used is：Metallic sodium, metallic potassium, germanium tetrachloride, toluene, ethyl alcohol, deionized water, a combination thereof
It is as follows to prepare dosage：It is measurement unit with gram, milliliter
Preparation method is as follows：
(1) selected chemical substance material
The chemical substance material that uses of preparation to be carried out selected, and carry out quality purity control：
(2) Na-K alloy is prepared
Metallic sodium 0.4g ± 0.03g is weighed, metallic potassium 1.6g ± 0.04g is weighed, 1min is stirred, at Na-K alloy；
(3) synthesising mesoporous germanium material
The synthesis of mesoporous germanium material is carried out under nitrogen protection, and reduction is first stirred at room temperature, and is obtained by filtration later solid
Body, finally high-temperature roasting under a nitrogen atmosphere.
1. preparing hybrid reaction mixture
2.4 ± 0.04g of germanium tetrachloride, 1.8 ± 0.03g of Na-K alloy are weighed, toluene 200mL ± 5mL is measured；
It is added in round-bottomed flask, at mixed reaction solution；
2. opening magnetic agitation, mixing time 4h, mixed reaction solution is reacted, and reaction equation is as follows：
GeCl4+ 4Na=4NaCl+Ge
GeCl4+ 4K=4KCl+Ge
3. after the completion of reaction, stopping stirring；Ethyl alcohol 100ml is added
(4) it filters
Mixture after reaction is placed in the Buchner funnel of bottle,suction, is filtered with miillpore filter, is retained on filter membrane
Product cake, waste liquid are evacuated in filter flask；
(5) it roasts
By the filter cake obtained by previous step in tubular type kiln roasting, temperature is 300-600 DEG C.
(6) it washs, filter
Product of roasting is placed in beaker, deionized water 100mL, agitator treating 5min is added；
Cleaning solution is placed in the Buchner funnel of bottle,suction, is filtered with miillpore filter, remaining product filter cake on filter membrane,
Cleaning solution is evacuated in filter flask；
Washing filters progress 2 times；
Product cake is placed in beaker, deionized water 100mL, agitator treating 5min is added；
Washing filters progress 2 times；
(7) it is dried in vacuo
Product cake after washing is placed in quartz container, is subsequently placed in vacuum drying chamber and is dried, dry temperature
50 DEG C ± 1 DEG C of degree, vacuum degree 50Pa, drying time 10h；
It is mesoporous germanium material after drying；
(8) test, analysis and characterization
The pattern, ingredient, Chemical Physics performance of the mesoporous germanium body material of preparation are detected, analyze, characterized；
The structural analysis of material is carried out with X-ray diffractometer；The results are shown in Figure 3, is the X-ray diffraction of mesoporous germanium material
Collection of illustrative plates, as it can be seen that gained germanium material has the structure of crystal in Fig. 3.
The pore passage structure analysis of material is carried out with nitrogen physisorption instrument；As shown in figure 4, being mesoporous germanium material nitrogen adsorption
Desorption curve figure, as it can be seen that gained germanium material has mesopore orbit structure in figure.
The Micro-Structure Analysis of material is carried out with transmission electron microscope；Shown in result figure 5, for mesoporous germanium material transmission electricity
Sub- microscope photo, as it can be seen that gained germanium material has pore passage structure in figure.Above-mentioned figure is carried out with material operating room software program
Graphics process；
(9) performance of lithium ion battery is studied
Active material, conductive carbon material and adhesive are with 70：15：15 ratio academic title's electrode solution slurries, are uniformly coated to
On copper foil.Electrochemical properties obtain polypropylene screens as diaphragm by CR2016 type button cells, and lithium foil is used as will to electrode
1mol L-1LiPF6(volume ratio 1 is dissolved in the mixed solution of diethyl carbonate, ethylene carbonate and dimethyl carbonate:1∶1)
With fluorinated ethylene carbonate (FEC, volume fraction 10%) as electrolysis additive batteries 0.01-1.50V constant electricity
Flow down cycle.
The conclusion obtained is：Synthesis germanium material is black powder at room temperature, and material has mesopore orbit structure, products collection efficiency
It is 95.2%；
(10) product storage
The mesoporous germanium material of preparation is stored in the glass container of amber transparent, it is closed to be kept in dark place, it waterproof, prevent
Damp, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C ± 2 DEG C of storage temperature, relative humidity≤10%.
It is cycle performance of the mesoporous germanium material as lithium ion battery negative material shown in Fig. 6, as it can be seen that gained germanium in Fig. 6
Material shows preferable chemical property when as lithium ion battery negative material.
Although having been combined the preferred embodiment of the present invention above shows that the present invention, those skilled in the art will
It will be appreciated that without departing from the spirit and scope of the present invention, can carry out various modifications, replace and change to the present invention
Become.Therefore, the present invention should not be limited by above-described embodiment, and should be limited by appended claims and its equivalent.
Claims (5)
1. a kind of preparation method of mesoporous germanium material, which is characterized in that the chemical substance material that this method includes is：Metallic sodium,
Metallic potassium, germanium tetrachloride, toluene, ethyl alcohol, deionized water；
A combination thereof dosage is as follows：It is measurement unit with gram, milliliter,
The synthesis of mesoporous germanium material is carried out in closed reactor, at room temperature, is completed during magnetic agitation；
Preparation method includes the following steps：
(1) Na-K alloy is prepared：Metallic sodium 0.4g ± 0.03g is weighed, metallic potassium 1.6g ± 0.04g is weighed, stirs 1min, configuration
At Na-K alloy；
(2) synthesising mesoporous germanium material：Under nitrogen protection, reduction is first stirred at room temperature, solid is obtained by filtration later, finally exists
High-temperature roasting under condition of nitrogen gas, obtains product of roasting；
(3) it washs, filter：
(4) it is dried in vacuo：It is mesoporous germanium material after drying；
(5) test, analysis and characterization：The pattern, ingredient, Chemical Physics performance of the mesoporous germanium body material of preparation are detected, divided
Analysis, characterization.
2. a kind of preparation method of mesoporous germanium material according to claim 1, which is characterized in that step (2) specifically includes
It is as follows：
A, hybrid reaction mixture is prepared：2.4 ± 0.04g of germanium tetrachloride, 1.8 ± 0.03g of Na-K alloy are weighed, toluene is measured
200mL ± 5mL is added in round-bottomed flask, at mixed reaction solution；
B, magnetic agitation, mixing time 4h are opened, mixed reaction solution is reacted, and reaction equation is as follows：
GeCl4+ 4Na=4NaCl+Ge
GeCl4+ 4K=4KCl+Ge
C, after the completion of reaction, stop stirring, ethyl alcohol 100ml is added；It filters：Mixture after reaction is placed in the Bu Shi of bottle,suction
It in funnel, is filtered with miillpore filter, remaining product filter cake waste liquid is evacuated in filter flask on filter membrane；Roasting：By the filter cake of gained
In tubular type kiln roasting, temperature is 300-600 DEG C.
3. a kind of preparation method of mesoporous germanium material according to claim 1, which is characterized in that step (3) washing,
Filter the specific steps are：Product of roasting is placed in beaker, deionized water 100mL, agitator treating 5min is added；By cleaning solution
It is placed in the Buchner funnel of bottle,suction, is filtered with miillpore filter, remaining product filter cake on filter membrane, cleaning solution is evacuated to filter flask
In, washing filters progress 2 times；Product cake is placed in beaker, deionized water 100mL, agitator treating 5min is added, wash,
It filters and carries out 2 times.
4. a kind of preparation method of mesoporous germanium material according to claim 1, which is characterized in that step (4) vacuum
It is dry the specific steps are：Product cake after washing is placed in quartz container, is subsequently placed in vacuum drying chamber and is done
It is dry, 50 DEG C ± 1 DEG C of drying temperature, vacuum degree 50Pa, drying time 10h.
5. mesoporous germanium material prepared by a kind of preparation method according to claim 1, which is characterized in that its can be applied to lithium from
Sub- cell negative electrode material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111270089A (en) * | 2020-01-20 | 2020-06-12 | 沈阳师范大学 | Mesoporous antimony material and preparation method thereof |
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| CN1706577A (en) * | 2005-04-28 | 2005-12-14 | 浙江大学 | Supersonic liquid phase reduction process for preparing monodisperse nano germanium crystal |
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| CN111270089A (en) * | 2020-01-20 | 2020-06-12 | 沈阳师范大学 | Mesoporous antimony material and preparation method thereof |
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