CN105655556B - A kind of preparation method of nanoporous antimony nickel alloy - Google Patents
A kind of preparation method of nanoporous antimony nickel alloy Download PDFInfo
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- CN105655556B CN105655556B CN201610027937.7A CN201610027937A CN105655556B CN 105655556 B CN105655556 B CN 105655556B CN 201610027937 A CN201610027937 A CN 201610027937A CN 105655556 B CN105655556 B CN 105655556B
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- antimony
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- potassium cyanide
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
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Abstract
The invention discloses a kind of preparation methods of nanoporous antimony nickel alloy, antimony trichloride and nickel potassium cyanide are dissolved in organic solvent respectively and form certain density solution, the solution of antimony trichloride and nickel potassium cyanide is mixed by certain molar ratio again, forms antimony trichloride/nickel potassium cyanide organic solvent gel；Using above-mentioned organic solvent gel as presoma, equivalent or excessive reducing agent are added thereto, reacts 0.1~24 hour, product is washed and dried, obtains the nanoporous antimony nickel alloy.The present invention prepares nanoporous antimony nickel alloy using antimony trichloride/nickel potassium cyanide organic solvent gel as presoma, the nanoporous antimony nickel alloy has three-dimensional porous network structure, there is structure and composition advantage simultaneously as lithium/anode material of lithium-ion battery, show preferably to store up lithium/sodium performance to meet the needs of power battery.
Description
Technical field
The present invention relates to a kind of preparation methods of lithium/anode material of lithium-ion battery, and in particular to a kind of nanoporous antimony
The preparation method of nickel alloy.As lithium ion and anode material of lithium-ion battery, the nanoporous antimony nickel alloy has only
Special structure and composition characteristic, shows preferably to store up lithium/sodium performance to meet the needs of power battery.
Background technology
Currently, the whole world is faced with two big severe challenge of energy crisis and environmental pollution.As high performance electrochmical power source,
Lithium/sodium-ion battery has that energy density is high, have extended cycle life, memory-less effect, self-discharge rate are low and advantages of environment protection,
It is considered as the ideal chose for the high-energy of traffic and energy storage field, high-power power battery, for the efficient profit of the energy
With, reduce carbon emission and environmental protection and have great importance.However, the specific capacity of Current commercial carbon negative pole material is relatively low,
Such as the theoretical specific capacity of graphite storage lithium is only 372mAh/g, lower specific capacity has seriously restricted lithium/sodium-ion battery and has made
For power battery traffic and energy storage field extensive use.
Metallic antimony (Sb) has many advantages, such as that alloy-type stores up lithium/sodium mechanism, has specific capacity height and safety good, is expected to replace
Be commercialized carbon-based material and as lithium/sodium ion power battery negative material.The storage lithium and storage sodium machine of metallic antimony negative material
System is as follows： The process of this alloy/removal alloying can
To bring high specific capacity, but can also cause huge volume change simultaneously, cause antimony sill dusting and specific capacity it is fast
Speed decaying.
Currently, research work, which is concentrated on, designs in terms of the structure and composition two of antimony sill and then improves its storage
Lithium/sodium performance.On the one hand, nano-porous structure has a nanometer module units, micron frame and porous characteristic, thus energy simultaneously
Show good structural stability and charge transport ability；On the other hand, by antimony and transition metal especially metallic nickel shape
At alloy, it can effectively buffer the volume change of antimony using inert metal nickel component and improve the electric conductivity of electrode material, to
Storage lithium/sodium performance of antimony material can be improved.Therefore, nanoporous antimony nickel alloy as lithium/anode material of lithium-ion battery simultaneously
With structure and composition advantage, it is expected to show preferably to store up lithium/sodium performance to meet the needs of power battery.
However related antimony nickel alloy, current report is concentrated mainly on prepares zero dimension antimony nickel alloy nanometer using solvent-thermal method
Crystalline substance includes that prodigious challenge is still suffered from the preparation of antimony nickel alloy in nanoporous antimony-containing alloy, and this restrict antimony-containing alloys
Include commercial applications of the antimony nickel alloy in lithium/anode material of lithium-ion battery.Therefore, seek to prepare the new side of antimony nickel alloy
Method has become a top priority.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of nanoporous antimony nickel alloy.As lithium ion and sodium ion
Cell negative electrode material, the nanoporous antimony nickel alloy have unique structure and composition characteristic, show preferably to store up lithium/sodium
It can be to meet the needs of power battery.
Completing the technical solution of foregoing invention task is：
A kind of preparation method of nanoporous antimony nickel alloy, it is characterised in that：Antimony trichloride and nickel potassium cyanide difference is molten
Solution is formed in organic solvent, then the solution of antimony trichloride and nickel potassium cyanide is mixed, it is organic to form antimony trichloride/nickel potassium cyanide
Sol gel；Using the organic solvent gel as presoma, equivalent or excessive reducing agent, reaction 0.1~24 are added thereto
Hour, product is washed and dried, the nanoporous antimony nickel alloy is obtained.
More specifically, the preparation method of nanoporous antimony nickel alloy of the invention, includes the following steps：
(1) preparation of antimony trichloride/nickel potassium cyanide organic solvent gel：Antimony trichloride and nickel potassium cyanide are dissolved in respectively to be had
Solvent forms certain density solution, then the solution of antimony trichloride and nickel potassium cyanide is mixed by certain molar ratio, is formed
Antimony trichloride/nickel potassium cyanide organic solvent gel；
(2) preparation of nanoporous antimony nickel alloy：The antimony trichloride obtained with step (1)/nickel potassium cyanide organic solvent is solidifying
Glue is presoma, and equivalent or excessive reducing agent are added thereto, reacts 0.1~24 hour, product is washed and dried, is obtained
The nanoporous antimony nickel alloy.
The organic solvent is dimethylformamide (DMF), tetrahydrofuran (THF), ethylene glycol (EG) and a contracting diethyl two
One or more of alcohol (DEG).
A concentration of 0.01~10 mol/L of the antimony trichloride in organic solvent, nickel potassium cyanide is in organic solvent
A concentration of 0.01~10 mol/L.
The molar ratio of the antimony trichloride and nickel potassium cyanide is 0.1:1~10:1.
The reducing agent is sodium borohydride, hydrazine hydrate or sodium hypophosphite etc..
Nanoporous antimony nickel alloy made from the method has three-dimensional porous network structure.Three-dimensional porous network structure
Average pore size is 2 nanometers~50 nanometers.
It compares and the prior art, the present invention has technique effect beneficial below：
(1) using antimony trichloride/nickel potassium cyanide organic solvent gel as presoma, which has mutual the present invention
Even spacial framework, Sb and Ni species are evenly distributed in the form of cyano bridging key on the interconnection skeleton of gel rubber system, bone
There are abundant nano apertures inside frame；In subsequent reduction process, the metallic antimony of generation can mutually be interconnected with nickel along gel skeleton
It connects and forms nanoporous antimony nickel alloy, overcome nanoporous antimony-containing alloy, include the preparation problem of antimony nickel alloy.
(2) present invention is by controlling antimony trichloride and nickel potassium cyanide concentration in organic solvent and antimony trichloride and nickel
The molar ratio of potassium cyanide can adjust the physical chemistry such as aperture and the composition of antimony trichloride/nickel potassium cyanide organic solvent gel
Matter, to further regulation and control nanoporous antimony nickel alloy aperture and group grade micro-structural properties and storage lithium and storage sodium
Energy.
(3) preparation process of the present invention is easy quickly, and large-scale production may be implemented.
Description of the drawings
Fig. 1：The transmission electron microscope picture of nanoporous antimony nickel alloy made from embodiment 1.
Fig. 2：The graph of pore diameter distribution of nanoporous antimony nickel alloy made from embodiment 1.
Fig. 3：The X-ray diffractogram of nanoporous antimony nickel alloy made from embodiment 1.
Fig. 4：The cycle performance figure of nanoporous antimony nickel alloy made from embodiment 1.
Fig. 5：The transmission electron microscope picture of nanoporous antimony nickel alloy made from embodiment 2.
Fig. 6：The graph of pore diameter distribution of nanoporous antimony nickel alloy made from embodiment 2.
Specific implementation mode
With reference to specific embodiment, the present invention will be described in detail.Protection scope of the present invention is not with specific implementation
Mode is limited, but is defined in the claims.
Embodiment 1：
(1) it antimony trichloride and nickel potassium cyanide is dissolved in dimethylformamide respectively forms a concentration of 5 mol/L and 0.5 and rub
You/liter solution, then the solution of antimony trichloride and nickel potassium cyanide is mixed, it is solidifying to form antimony trichloride/nickel potassium cyanide organic solvent
Glue, wherein the molar ratio of antimony trichloride and nickel potassium cyanide is 1:1.
(2) antimony trichloride obtained using step (1)/nickel potassium cyanide organic solvent gel was added thereto as presoma
The reducing agent sodium borohydride of amount reacts 1 hour, product is washed and dried, and obtains the nanoporous antimony nickel alloy.
From transmission electron microscope picture as it can be seen that product has typical nano-porous structure, and the nano-porous structure is by nanometer
The network structure that particle is interconnected to form on three-dimensional has abundant nano-pore in inside configuration；By aperture point
Butut is as it can be seen that the average pore size of porous network structure is 14.1 nanometers；X ray diffracting spectrum shows that the crystalline phase of antimony nickel alloy is
Single hexagonal phase NiSb intermetallic compounds；As lithium ion battery negative material, which shows
Good cyclical stability；After 180 cycles, reversible specific capacity is still up to 425.4mA h g-1, it is higher than business graphite
Theoretical specific capacity (the 372mA h g of negative material-1), thus the practical prospect shown.
Embodiment 2：
(1) it antimony trichloride and nickel potassium cyanide is dissolved in dimethylformamide respectively forms a concentration of 5 mol/L and 0.5 and rub
You/liter solution, then the solution of antimony trichloride and nickel potassium cyanide is mixed, it is solidifying to form antimony trichloride/nickel potassium cyanide organic solvent
Glue, wherein the molar ratio of antimony trichloride and nickel potassium cyanide is 4:1.
(2) antimony trichloride obtained using step (1)/nickel potassium cyanide organic solvent gel was added thereto as presoma
The reducing agent sodium borohydride of amount reacts 1 hour, product is washed and dried, and obtains the nanoporous antimony nickel alloy.
Its result and embodiment 1 are similar.By transmission electron microscope picture as it can be seen that product has typical three-dimensional porous network structure；
By graph of pore diameter distribution as it can be seen that the average pore size of porous network structure is 11.8 nanometers.
Embodiment 3：
(1) antimony trichloride and nickel potassium cyanide are dissolved in tetrahydrofuran respectively and form a concentration of 1 mol/L and 0.1 mol/L
Solution, then by the solution of antimony trichloride and nickel potassium cyanide mix, formed antimony trichloride/nickel potassium cyanide organic solvent gel,
In, the molar ratio of antimony trichloride and nickel potassium cyanide is 2:1.
(2) antimony trichloride obtained using step (1)/nickel potassium cyanide organic solvent gel is presoma, addition etc. thereto
The reducing agent hydrazine hydrate of amount reacts 6 hours, product is washed and dried, and obtains the nanoporous antimony nickel alloy.
Its result and embodiment 1 are similar.
Embodiment 4：
(1) by antimony trichloride and nickel potassium cyanide be dissolved in respectively diglycol formed a concentration of 0.01 mol/L and
The solution of 0.01 mol/L, then the solution of antimony trichloride and nickel potassium cyanide is mixed, it is organic to form antimony trichloride/nickel potassium cyanide
Sol gel, wherein the molar ratio of antimony trichloride and nickel potassium cyanide is 1:2.
(2) antimony trichloride obtained using step (1)/nickel potassium cyanide organic solvent gel was added thereto as presoma
The reducing agent sodium hypophosphite of amount reacts 12 hours, product is washed and dried, and obtains the nanoporous antimony nickel alloy.
Its result and embodiment 1 are similar.
Embodiment 5：
(1) antimony trichloride is dissolved in the solution that dimethylformamide forms a concentration of 0.1 mol/L, nickel potassium cyanide is dissolved in
Ethylene glycol forms the solution of a concentration of 0.2 mol/L, then the solution of antimony trichloride and nickel potassium cyanide is mixed, and forms tri-chlorination
Antimony/nickel potassium cyanide organic solvent gel, wherein the molar ratio of antimony trichloride and nickel potassium cyanide is 0.1:1.
(2) antimony trichloride obtained using step (1)/nickel potassium cyanide organic solvent gel is presoma, addition etc. thereto
The reducing agent sodium borohydride of amount reacts 0.1 hour, product is washed and dried, and obtains the nanoporous antimony nickel alloy.
Its result and embodiment 1 are similar.
Embodiment 6：
(1) antimony trichloride is dissolved in the solution that ethylene glycol forms a concentration of 10 mol/L, nickel potassium cyanide is dissolved in a contracting diethyl
Glycol forms the solution of a concentration of 1 mol/L, then the solution of antimony trichloride and nickel potassium cyanide is mixed, and forms antimony trichloride/nickel
Potassium cyanide organic solvent gel, wherein the molar ratio of antimony trichloride and nickel potassium cyanide is 10:1.
(2) antimony trichloride obtained using step (1)/nickel potassium cyanide organic solvent gel was added thereto as presoma
The reducing agent sodium borohydride of amount reacts 24 hours, product is washed and dried, and obtains the nanoporous antimony nickel alloy.
Its result and embodiment 1 are similar.
Claims (6)
1. a kind of preparation method of nanoporous antimony nickel alloy, which is characterized in that include the following steps：
(1) preparation of antimony trichloride/nickel potassium cyanide organic solvent gel：Antimony trichloride and nickel potassium cyanide are dissolved in respectively organic molten
For dosage form at certain density solution, the organic solvent is dimethylformamide, tetrahydrofuran, ethylene glycol and diglycol
One or more of；The solution of antimony trichloride and nickel potassium cyanide is mixed by certain molar ratio again, forms antimony trichloride/nickel
Potassium cyanide organic solvent gel；
(2) preparation of nanoporous antimony nickel alloy：The antimony trichloride obtained with step (1)/nickel potassium cyanide organic solvent gel is
Equivalent or excessive reducing agent is added in presoma thereto, reacts 0.1~24 hour, product is washed and dried, and obtains described
Nanoporous antimony nickel alloy.
2. the preparation method of nanoporous antimony nickel alloy according to claim 1, it is characterised in that：The antimony trichloride exists
A concentration of 0.01~10 mol/L in organic solvent, nickel potassium cyanide in organic solvent a concentration of 0.01~10 mole/
It rises.
3. the preparation method of nanoporous antimony nickel alloy according to claim 1, it is characterised in that：The antimony trichloride with
The molar ratio of nickel potassium cyanide is 0.1:1~10:1.
4. the preparation method of nanoporous antimony nickel alloy according to claim 1, it is characterised in that the reducing agent is boron
Sodium hydride, hydrazine hydrate or sodium hypophosphite.
5. the preparation method of nanoporous antimony nickel alloy according to claim 1, it is characterised in that the method is prepared into
The nanoporous antimony nickel alloy arrived has three-dimensional porous network structure.
6. the preparation method of nanoporous antimony nickel alloy according to claim 5, it is characterised in that described is three-dimensional porous
The average pore size of network structure is 2 nanometers~50 nanometers.
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| CN108807850B (en) * | 2017-05-01 | 2021-08-27 | 深圳格林德能源集团有限公司 | Electrode and sodium ion battery |
| CN108927154A (en) * | 2018-06-11 | 2018-12-04 | 大连理工大学 | A kind of preparation method of intermetallic compound nanocatalyst |
| 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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| CN103290246A (en) * | 2013-05-27 | 2013-09-11 | 南京师范大学 | Preparation method of three-dimensional nano porous tin-base alloy for lithium-ion battery negative electrode |
| CN105195757A (en) * | 2014-06-23 | 2015-12-30 | 巴莱诺斯清洁能源控股公司 | Sb nanocrystals or Sb-alloy nanocrystals for fast charge/discharge Li- and Na-ion battery anodes |
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| CN103290246A (en) * | 2013-05-27 | 2013-09-11 | 南京师范大学 | Preparation method of three-dimensional nano porous tin-base alloy for lithium-ion battery negative electrode |
| CN105195757A (en) * | 2014-06-23 | 2015-12-30 | 巴莱诺斯清洁能源控股公司 | Sb nanocrystals or Sb-alloy nanocrystals for fast charge/discharge Li- and Na-ion battery anodes |
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