CN109837610A - A kind of Na2TiSiO5The electrostatic spinning preparation method of C nano fiber - Google Patents
A kind of Na2TiSiO5The electrostatic spinning preparation method of C nano fiber Download PDFInfo
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- CN109837610A CN109837610A CN201910144472.7A CN201910144472A CN109837610A CN 109837610 A CN109837610 A CN 109837610A CN 201910144472 A CN201910144472 A CN 201910144472A CN 109837610 A CN109837610 A CN 109837610A
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Abstract
The invention discloses a kind of Na2TiSiO5The electrostatic spinning preparation method of C nano fiber.First ethyl orthosilicate, butyl titanate is added in n,N-Dimethylformamide, ethyl alcohol and acetic acid after mixing, adds sodium propionate magnetic and stir to being completely dissolved, obtain light yellow transparent solution;Polyvinylpyrrolidone is added, continues to stir, obtains the electrostatic spinning precursor solution of pale yellow transparent.Precursor solution is transferred in electrostatic spinning injector for medical purpose, the spinning on electrostatic spinning apparatus is started, the nanofiber that spinning obtains is received with tinfoil paper.The tinfoil paper substrate for being loaded with nanofiber is first dried in vacuo later, then carries out carbonization treatment, obtains final black product Na2TiSiO5C nano fiber.Gained Na of the invention2TiSiO5C nano fibre diameter is uniform, about 150~200nm, has excellent chemical property.
Description
Technical field
The present invention relates to a kind of anode material of lithium-ion battery, in particular to a kind of Na2TiSiO5The electrostatic of C nano fiber
Spinning preparation method.
Background technique
Environmental pollution increasingly severe today, dependence of the human development to fossil fuel is gradually got rid of, the earth is improved
Ecological environment becomes the common recognition of today's society.The renewable and clean energy resources such as solar energy, wind energy, tide energy become the following replacementization
The main energy sources of stone fuel support progress of human society, and how to store these energy and developed as entire energy field
Important link in journey.Lithium ion battery is excellent with high-energy density, high voltage, low self discharge and excellent cycle performance etc.
Gesture becomes the main energy storage device of consumer electronics field.But global more deficient (the abundance deficiency in the earth's crust of lithium resource
0.0007%) it, is unevenly distributed, lithium source, which holds at high price, becomes an important factor for limiting its development.And since sodium and lithium are in
Same main group has similar electrochemical properties, and sodium has great economic advantages, and the abundance in the earth's crust reaches
2.6%, therefore, sodium-ion battery becomes current popular energy storage system.
Numerous negative electrode materials suitable for sodium-ion battery, titanium base material is with environmental-friendly, stability is good, safety
The good advantage of property, causes people and largely pays close attention to and study.Titanium silicate sodium (Na2TiSiO5) it is considered as most potential sodium
One of negative electrode material of ion battery.
In recent years, electrostatic spinning technique is since equipment is simple, the easily-controllable extensive concern for causing scientific research personnel of preparation process,
It is considered as preparing one of nanofiber most simple effective method.Electrostatic spinning is polymer solution or melt in electrostatic interaction
The lower method for carrying out injection stretching and obtaining nano-scale fiber, easily prepared homogenous composite, such as doping, functionalization
Deng, and the material specific surface area with higher being prepared and biggish draw ratio.Just because of these unique advantages,
Electrostatic spinning technique can be applied in many fields such as the energy, environment, biomedicine.Currently, report is mainly mostly
Li2TiSiO5The research of-C negative electrode material, and to Na2TiSiO5The electrostatic spinning of C nano fiber prepares and the report of storage sodium performance
Road is rare.Therefore, Na is prepared using electrostatic spinning2TiSiO5C nano fiber has very important significance.
Summary of the invention
For the Na of the prior art2TiSiO5The problems such as-C preparation process is complicated, the present invention provide a kind of simple process, property
The excellent Na of energy2TiSiO5The electrostatic spinning preparation method of C nano fiber.
The technical solution of the present invention is as follows:
A kind of Na2TiSiO5The electrostatic spinning preparation method of C nano fiber, includes the following steps:
(1) n,N-Dimethylformamide, ethyl alcohol are uniformly mixed with acetic acid, obtain mixed solvent, add positive silicic acid second
Then ester and butyl titanate are added sodium propionate and stir the solution for obtaining pale yellow transparent to being completely dissolved;
(2) polyvinylpyrrolidone is added into step (1) acquired solution, continues to stir, obtains the quiet of pale yellow transparent
Electrospun precursor solution;
(3) precursor solution obtained by step (2) is transferred in electrostatic spinning injector for medical purpose, is started in electrostatic spinning
Spinning on device, the nanofiber that spinning obtains are received with tinfoil paper;
(4) the substrate tinfoil paper for being loaded with nanofiber resulting to step (3) is first dried, and then carries out carbonization treatment,
Obtain final black product, i.e. Na2TiSiO5C nano fiber.
Further, the in the mixed solvent in step (1), the volume ratio of n,N-Dimethylformamide, ethyl alcohol and acetic acid are 8
~9:2~13:1~2.
Further, in step (1), the volume ratio of ethyl orthosilicate, butyl titanate and mixed solvent is 1~2:1~2:
26~27.
Further, in step (1), the mass ratio of sodium propionate and mixed solvent is 1~1.5:39~40.
Further, the polyvinylpyrrolidone average molecular weight in step (1) is 1300000.
Further, in step (2), the additional amount of polyvinylpyrrolidone be step (1) acquired solution quality 7.0~
8.66%.
Further, the electrospinning parameters in step (3) are as follows: the spacing between spinning syringe needle and metal collection substrate is
15~18cm, spinning voltage are 15~18KV, and environment temperature is 30~60 DEG C, and humidity is about 20~40%, is to liquid speed degree
0.2~0.5mL/h.
Further, the drying of step (4) is vacuum drying, and drying temperature is 60~80 DEG C, and drying time is 4~6h.
Further, the carbonization treatment of step (4) is to collect nanofiber with corundum Noah's ark to be put into logical Ar air-tube type furnace
Calcining, detailed process are to be raised to 800~900 DEG C with the heating rate of 4 DEG C/min from room temperature, kept the temperature 3~4h.
It is worth noting that each factor synergistic effect in present invention process, be finally obtained the product of function admirable, it is each because
Element is indispensable, for example, experiment shows that the mixed solvent that the present invention uses is made of by a certain percentage three kinds of substances, the mixing
Solvent has played very important effect in process, if it is bulk that the product that acetic acid obtains is not added in solvent, at this point, finally
Resulting product be not it is nanometer fibrous, performance is far away from Na2TiSiO5C nano fiber.
The present invention has the following technical effect that:
Preparation process of the present invention is simple and convenient to operate, gained Na2TiSiO5C nano fiber is a kind of novel, simple electricity
Pond negative electrode material.Na prepared by the present invention2TiSiO5C nano fibrous material uniform diameter, about 150~200nm have excellent
Chemical property, high rate performance and cycle performance are very good.
Detailed description of the invention
Fig. 1 is Na prepared by the embodiment of the present invention 12TiSiO5The scanning electron microscope (SEM) photograph of-C bulk material.
Fig. 2 is Na prepared by the embodiment of the present invention 52TiSiO5The scanning electron microscope (SEM) photograph of C nano fiber.
Fig. 3 is Na prepared by the embodiment of the present invention 52TiSiO5The x-ray diffraction pattern of C nano fiber.
Fig. 4 is Na prepared by the embodiment of the present invention 52TiSiO5For C nano fiber as negative electrode material, metallic sodium piece is pair
Electrode is assembled into button cell.At 20~25 DEG C, in the voltage range of 0.01~2.5V, different current densities 10,20,50,
100,200,500,1000,2000 and 10mA g-1The lower high rate performance figure and coulombic efficiency figure for carrying out charge-discharge test.
Fig. 5 is Na prepared by the embodiment of the present invention 52TiSiO5For C nano fiber as negative electrode material, metallic sodium piece is pair
Electrode is assembled into button cell.At 20~25 DEG C, in the voltage range of 0.01~2.5V, 20mA g-1Current density under into
The cycle life and coulombic efficiency figure of row charge-discharge test.
Specific embodiment
The present invention will be further described combined with specific embodiments below, but the present invention is not limited thereto.
Embodiment 1
At 15~25 DEG C, it is added in the salable vial equipped with 6mL n,N-Dimethylformamide and 4mL ethyl alcohol
The butyl titanate of the ethyl orthosilicate of 0.3mL, 0.5mL, solution is added after mixing in magnetic agitation 5min at 300 rpm
The sodium propionate of 0.264g continues stirring 5min and obtains light yellow transparent solution;The polyvinylpyrrolidone for adding 0.8g,
6h is stirred under the revolving speed of 300rpm;Obtained light yellow transparent solution is transferred in electrostatic spinning injector for medical purpose, is started
The spinning on electrostatic spinning apparatus, the nanofiber that spinning obtains are received with tinfoil paper.Electrospinning parameters are as follows: spinning syringe needle and gold
Belonging to the spacing collected between substrate is 15cm, and spinning voltage 15KV, environment temperature is 30 DEG C, and humidity is about 30%, gives liquid
Speed is 0.18mL/h.The substrate tinfoil paper of nanofiber is loaded in 60 DEG C of vacuum drying 6h, collects the Nanowire on substrate tinfoil paper
Dimension moves into corundum Noah's ark, is put into logical Ar air-tube type furnace and is sintered annealing, and specific calcination process is that 200 DEG C are raised to from room temperature, protects
Warm 2h, then 850 DEG C are warming up to, 4h is kept the temperature, is cooled to room temperature the blocky Na up to black later2TiSiO5C-material.
Embodiment 2
At 15~25 DEG C, can be close with 1mL acetic acid mixed solution equipped with 6mL n,N-Dimethylformamide, 4mL ethyl alcohol
The butyl titanate of ethyl orthosilicate, 0.5mL that 0.3mL is added, the magnetic agitation 5min under the revolving speed of 300rpm are sealed in vial
The sodium propionate for making solution that 0.264g be added after mixing continues to stir 5min, obtains light yellow transparent solution;Add 0.8g
Polyvinylpyrrolidone, stir 6h under the revolving speed of 300rpm;Obtained light yellow transparent solution is transferred to electrostatic spinning
With in injector for medical purpose (flat mouth syringe needle), start the spinning on electrostatic spinning apparatus, the nanofiber that spinning obtains is connect with tinfoil paper
It receives.Electrospinning parameters are as follows: the spacing between spinning syringe needle and metal collection substrate is 15cm, spinning voltage 15KV, environment
Temperature is 30 DEG C, and humidity is about 30%, is 0.18mL/h to liquid speed degree.The substrate tinfoil paper of nanofiber is loaded in 60 DEG C of vacuum
Dry 6h, the nanofiber collected on substrate tinfoil paper move into corundum Noah's ark, are put into logical Ar air-tube type furnace and are sintered annealing, specifically
Calcination process is that 200 DEG C are raised to from room temperature, keeps the temperature 2h, then be warming up to 850 DEG C, keeps the temperature 4h, is cooled to room temperature later up to black
Na2TiSiO5C nano fibrous material.
Embodiment 3
At 15~25 DEG C, equipped with 5mL n,N-Dimethylformamide, 5mL ethyl alcohol and 0.5mL acetic acid mixed solution can
The ethyl orthosilicate of 0.3mL, the butyl titanate of 0.5mL are added in sealed glass jars, magnetic agitation 5min makes molten at 300 rpm
The sodium propionate that 0.264g is added in liquid after mixing continues to stir 5min, obtains light yellow transparent solution;Add the poly- of 0.8g
Vinylpyrrolidone stirs 6h under the revolving speed of 300rpm;Obtained light yellow transparent solution is transferred to electrostatic spinning doctor
With in syringe, start the spinning on electrostatic spinning apparatus, the nanofiber that spinning obtains is received with tinfoil paper.Electrospinning parameters
Are as follows: the spacing between spinning syringe needle and metal collection substrate is 15cm, and spinning voltage 15KV, environment temperature is 30 DEG C, humidity
About 30%, it is 0.18mL/h to liquid speed degree.The substrate tinfoil paper of nanofiber is loaded in 60 DEG C of vacuum drying 6h, collects substrate
Nanofiber on tinfoil paper moves into corundum Noah's ark, is put into logical Ar air-tube type furnace and is sintered annealing, and specific calcination process is from room
Temperature rise keeps the temperature 2h to 200 DEG C, then is warming up to 850 DEG C, keeps the temperature 4h, is cooled to room temperature the Na up to black later2TiSiO5- C receives
Rice fibrous material.
Embodiment 4
At 15~25 DEG C, equipped with 6mL n,N-Dimethylformamide, 4mL ethyl alcohol and 0.5mL acetic acid mixed solution can
The ethyl orthosilicate of 0.3mL, the butyl titanate of 0.5mL are added in sealed glass jars, magnetic agitation 5min makes molten at 300 rpm
The sodium propionate that 0.264g is added in liquid after mixing continues to stir 5min, obtains light yellow transparent solution;Add the poly- of 1.0g
Vinylpyrrolidone stirs 6h under the revolving speed of 300rpm;Obtained light yellow transparent solution is transferred to electrostatic spinning doctor
With in syringe, start the spinning on electrostatic spinning apparatus, the nanofiber that spinning obtains is received with tinfoil paper.Electrospinning parameters
Are as follows: the spacing between spinning syringe needle and metal collection substrate is 15cm, and spinning voltage 15KV, environment temperature is 30 DEG C, humidity
About 30%, it is 0.18mL/h to liquid speed degree.The substrate tinfoil paper of nanofiber is loaded in 60 DEG C of vacuum drying 6h, collects substrate
Nanofiber on tinfoil paper moves into corundum Noah's ark, is put into logical Ar air-tube type furnace and is sintered annealing, and specific calcination process is from room
Temperature rise keeps the temperature 2h to 200 DEG C, then is warming up to 850 DEG C, keeps the temperature 4h, is cooled to room temperature the Na up to black later2TiSiO5- C receives
Rice fibrous material.
Embodiment 5
At 15~25 DEG C, equipped with 6mL n,N-Dimethylformamide, 4mL ethyl alcohol and 0.5mL acetic acid mixed solution can
The ethyl orthosilicate of 0.3mL, the butyl titanate of 0.5mL are added in sealed glass jars, magnetic agitation 5min makes molten at 300 rpm
The sodium propionate that 0.264g is added in liquid after mixing continues to stir 5min, obtains light yellow transparent solution;Add the poly- of 0.8g
Vinylpyrrolidone stirs 6h under the revolving speed of 300rpm;Obtained light yellow transparent solution is transferred to electrostatic spinning doctor
With in syringe, start the spinning on electrostatic spinning apparatus, the nanofiber that spinning obtains is received with tinfoil paper.Electrospinning parameters
Are as follows: the spacing between spinning syringe needle and metal collection substrate is 15cm, and spinning voltage 15KV, environment temperature is 30 DEG C, humidity
About 30%, it is 0.18mL/h to liquid speed degree.The substrate tinfoil paper of nanofiber is loaded in 60 DEG C of vacuum drying 6h, collects substrate
Nanofiber on tinfoil paper moves into corundum Noah's ark, is put into logical Ar air-tube type furnace and is sintered annealing, and specific calcination process is from room
Temperature rise keeps the temperature 2h to 200 DEG C, then is warming up to 850 DEG C, keeps the temperature 4h, is cooled to room temperature the Na up to black later2TiSiO5- C receives
Rice fibrous material.
2 to 5 products obtained therefrom of embodiment is used for all kinds of characterizations and performance test, acquired results are almost the same, below with reality
It applies and is illustrated for 5 products obtained therefrom of example.
As shown in Fig. 2, it can be seen from the figure that Na obtained2TiSiO5C nano fibre diameter is uniform, about 150~
200nm, so as to be conducive to Na+Intercalation/deintercalation, have good chemical property.
As shown in Fig. 2, by with Na2TiSiO5Standard card PDF 46-1419 compare as can be seen that preparation
Na2TiSiO5C nano fibrous material and Na2TiSiO5Characteristic diffraction peak coincide very well, carbon therein is amorphous.
As shown in figure 4, with Na made from embodiment 52TiSiO5For C nano fiber as negative electrode material, metallic sodium piece is pair
Electrode is assembled into button cell.At 20~25 DEG C, in the voltage range of 0.01~2.5V, different current densities 10,20,50,
100,200,500,1000,2000 and 20,10mA g-1The lower high rate performance figure for carrying out charge-discharge test.In 10mA g-1's
Under current density, the specific discharge capacity after 5 circle of circulation is 101.6mAh g-1, when current density rises to 20,50,100,200,
500,1000 and 2000mAg-1When, specific discharge capacity is respectively 93.4,76.7,67.3,54.8,45.1,37.3 and
29.8mAh g-1, current density returns to 20mA g after the charge and discharge of super-high-current-1、10mA g-1When, be still respectively provided with 83.7,
88.7mAh g-1Specific discharge capacity, show Na2TiSiO5C nano fiber has good high rate performance.
As shown in figure 5, with Na made from embodiment 52TiSiO5For C nano fiber as negative electrode material, metallic sodium piece is pair
Electrode is assembled into button cell.At 20~25 DEG C, in the voltage range of 0.01~2.5V, 20mAg-1Current density under into
The test of row charge and discharge cycles, first discharge specific capacity are 367mAh g-1, charge specific capacity is 110mAh g-1;After circulation 100 times
Specific discharge capacity be 89.5mAh g-1, charge specific capacity is 87.3mAh g-1;Circulation 200 times after specific discharge capacity be
86.7mAh g-1, charge specific capacity is 84.7mAh g-1, show Na2TiSiO5C nano fibrous material has stable cyclicity
Energy.
Claims (9)
1. a kind of Na2TiSiO5The electrostatic spinning preparation method of C nano fiber, which comprises the steps of:
(1) n,N-Dimethylformamide, ethyl alcohol are uniformly mixed with acetic acid, obtain mixed solvent, add ethyl orthosilicate and
Then butyl titanate is added sodium propionate and stirs to being completely dissolved, obtains light yellow transparent solution;
(2) polyvinylpyrrolidone is added into step (1) acquired solution, continues to stir, obtains the Static Spinning of pale yellow transparent
Silk precursor solution;
(3) precursor solution obtained by step (2) is transferred in electrostatic spinning injector for medical purpose, is started on electrostatic spinning apparatus
Spinning, the nanofiber that spinning obtains are received with tinfoil paper;
(4) the substrate tinfoil paper for being loaded with nanofiber resulting to step (3) is first dried, and then carries out carbonization treatment, obtains
Final black product, i.e. Na2TiSiO5C nano fiber.
2. Na according to claim 12TiSiO5The electrostatic spinning preparation method of C nano fiber, which is characterized in that step
(1) in the mixed solvent in, the volume ratio of n,N-Dimethylformamide, ethyl alcohol and acetic acid are 8~9:12~13:1~2.
3. Na according to claim 12TiSiO5The electrostatic spinning preparation method of C nano fiber, which is characterized in that step
(1) in, the volume ratio of ethyl orthosilicate, butyl titanate and mixed solvent is 1~2:1~2:26~27.
4. Na according to claim 12TiSiO5The electrostatic spinning preparation method of C nano fiber, which is characterized in that step
(1) in, the mass ratio of sodium propionate and mixed solvent is 1~1.5:39~40.
5. Na according to claim 12TiSiO5The electrostatic spinning preparation method of C nano fiber, which is characterized in that step
(2) the polyvinylpyrrolidone average molecular weight in is 1300000.
6. Na according to claim 12TiSiO5The electrostatic spinning preparation method of C nano fiber, which is characterized in that step
(2) in, the additional amount of polyvinylpyrrolidone is the 7.0~8.66% of step (1) acquired solution quality.
7. Na according to claim 12TiSiO5The electrostatic spinning preparation method of C nano fiber, which is characterized in that step
(3) electrospinning parameters in are as follows: the spacing between spinning syringe needle and metal collection substrate is 15~18cm, spinning voltage 15
~18KV, environment temperature are 30~60 DEG C, and humidity is 20~40%, are 0.2~0.5mL/h to liquid speed degree.
8. Na according to claim 12TiSiO5The electrostatic spinning preparation method of C nano fiber, which is characterized in that step
(4) drying is vacuum drying, and drying temperature is 60~80 DEG C, and drying time is 4~6h.
9. Na according to claim 12TiSiO5The electrostatic spinning preparation method of C nano fiber, which is characterized in that step
(4) carbonization treatment in is to be put into logical Ar air-tube type furnace to calcine with corundum Noah's ark collection nanofiber, with the liter of 4 DEG C/min
Warm rate is raised to 800~900 DEG C from room temperature, keeps the temperature 3~4h.
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Application publication date: 20190604 |