CN106830058A - A kind of cellular tin dioxide material and preparation method thereof - Google Patents
A kind of cellular tin dioxide material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of preparation method of cellular tin dioxide material, belong to lithium (sodium) ion battery electrode materials preparing technical field, main purpose is to solve existing electrode material cyclical stability difference and the low problem of specific capacity.The method of the present invention comprises the steps：First, a certain proportion of tetraethyl orthosilicate, ethanol, water and ammoniacal liquor are mixed, is stirred at room temperature and obtains silicon oxide pellets；2nd, one layer of tin ash is grown on the silicon oxide pellets prepared by step one using hydro-thermal method；3rd, it is template glucose as carbon source with sodium chloride, high temperature cabonization obtains coating the carbon film of nanometer bead, using NaOH etching silicon dioxide, obtains cellular tin ash/carbon composite.Tin ash/carbon composite that the present invention is prepared using template, this material is demonstrated by the excellent chemical properties such as specific capacity and good cyclical stability higher in lithium (sodium) ion battery.
Description
Technical field
The invention belongs to material and electrochemical energy storing device field, more particularly, to a kind of cellular tin ash material
Material and preparation method thereof.
Background technology
As the modern life and industrial production are continuously increased to the demand of fossil fuel, the earth is faced with increasingly serious
Environmental problem, this also stimulate people explore can large-scale application clean reproducible energy, and for major part it is renewable
The energy, such as solar energy, wind energy etc. are all intermittent, therefore development high efficiency energy storage technology is to the big rule of regenerative resource
Mould application seems increasingly important.
Secondary lithium battery has obtained rapid development in recent years as a kind of excellent energy storage device, and wide
It is general to be applied in the middle of various portable electric appts and electric automobile, simultaneously as on the earth lithium reserves limitation, to sodium ion
The research and development of battery also receive more and more concerns.Therefore researching and developing high performance lithium (sodium) ion battery electrode materials seems especially heavy
Will.Compared with commercial graphite, tin ash has theoretical specific capacity higher, on tin ash as lithium (sodium) ion negative pole
The research of material is also compared many.But either during Lithium-ion embeding or sodium ion are embedded in, the volume of tin ash
Violent expansion will occur, and have a strong impact on the cyclical stability and multiplying power property of electrode material.In order to solve the above problems,
Generally it is that tin ash and carbon are combined and designed special microstructure by the way of.Because carbon not only can be with strengthening material
The electric conductivity of material can also play certain effect of contraction to the volumetric expansion of tin ash, and the design of special construction is favourable
Certain cushion space is provided in the expansion for material.Such as Lei Zhang etc. are prepared using a kind of method of selective etch
Porous SnO 2 hollow micro- cube structure, the advantage is that porous and hollow-core construction can provide more surfaces reaction positions
Point, but the volumetric expansion of simple tin dioxide material in charge and discharge process is severe, it is easy to and stability reunion is low, to material
Using bringing extreme difficulties (Energy Environ.Sci., 2014,7,1013-1017)；Jianping Li etc. use template
Method is prepared for the small spherical structure of nucleocapsid of tin ash/carbon, the advantage is that core shell structure provide not only certain cushion space,
Carbon coating layer also further avoid the reunion of tin ash simultaneously, for negative material provides reliable cyclical stability, so
And the dispersiveness of nanometer bead result in electronics or the obstacle of ion transmission in charge and discharge process, the performance to electrode material is outstanding
It is that multiplying power property produces certain influence (CrystEngComm, 2014,16,517).Advantage based on such scheme and lack
Point, this patent prepares high performance cellular tin ash lithium (sodium) ion battery negative pole there is provided advantage advantageously
Material.
The content of the invention
It is an object of the invention to provide a kind of reasonable design and cellular tin dioxide material with excellent properties and
Its preparation method, can prepare high-performance, and the more ion battery cathode material with favourable advantage.
The invention discloses a kind of preparation method of cellular tin dioxide material, it is characterised in that the method is included such as
Lower step：
Step one：The preparation of silicon oxide pellets
Take 60-70mL ethanol and 30-40mL deionized waters are uniformly mixed in same beaker, add 4-5mL's
The mass fraction of tetraethyl orthosilicate and 8-10mL is 25% ammoniacal liquor, is stirred at room temperature 8-12 hours, be centrifuged and spend from
Sub- water and alcohol are washed multiple and dried respectively；
Step 2：The preparation of tin ash coated silica bead
Weigh a kind of acquisition of the step 0.03-0.06g silicon oxide pellets and ultrasonic disperse 50-70mL water and
In alcohol mixeding liquid, wherein the volume fraction of ethanol is 37.5-45%；Add afterwards 0.3-0.4g facile hydrolysis pink salt and
1.2-1.8g urea and after continuously stirring 5-10 minutes, suspension is transferred in the water heating kettle of 100mL, at 160-180 DEG C
Product is obtained after reaction 12-18 hours, centrifuge washing and drying；
Step 3：The preparation of cellular tin dioxide material
Tin ash coated silica bead prepared by the step 2 is taken into 0.2-0.3g, ultrasonic disperse is in 50-
In 70mL deionized waters, the water soluble salt dissolving of 0.1-0.3g organic solutes and 8-10g cubics is added wherein；Heating
To seethe with excitement and be stirred continuously make moisture evaporating completely after obtain white powder, it is heated to 550- under the atmosphere of protective gas
700 DEG C and natural cooling after 2-3 hours is incubated, gains are dispersed in the NaOH of 2-3mol/L or hydrofluoric acid solution simultaneously
8-12 hour of immersion, filtration washing repeatedly and is dried.
Further, the pink salt of the facile hydrolysis is three hydrated stannic acid potassium, stannic chloride or stannous chloride or above-mentioned material
Hydrate.
Further, the organic solute is glucose, sucrose or citric acid.
Further, using the cellular tin dioxide material preparation method prepared by tin dioxide material.
Further, using the cellular tin dioxide material preparation method prepared by the lithium that is produced of material or
Anode material of lithium-ion battery.
Cellular tin ash lithium (sodium) ion battery cathode material prepared by the present invention, possesses the cellular of reasonable design
Novel structure.Nano silicon bead is employed as template, the small spherical structure of hollow tin ash is prepared, at the same using cube
Shape sodium chloride template obtains sheet carbon structure, finally gives hollow stannic oxide nanometer bead and is embedded in the middle of stratiform C film
There is holes in structure, the upper surface of some beads.Tin ash has theoretical specific capacity higher and designed in this structure
Tin ash bead can effectively be linked together and not only contribute to the electric conductivity of reinforcing material and can also preferably promote by carbon plate
Enter the transmission of electronics or ion, while tin ash bead is coated in the middle of carbon film can play certain limitation to its volumetric expansion
Effect, the cavity structure in tin ash bead also can provide certain cushion space for its volumetric expansion, therefore reasonably
Design causes that this electrode material shows very excellent chemical property in lithium (sodium) ion battery.
Brief description of the drawings
Fig. 1 is the preparation principle figure of cellular tin dioxide material provided in an embodiment of the present invention；
Fig. 2 is the XRD of the preparation cellular tin dioxide material of gained in the embodiment of the present invention；
Fig. 3 is the SEM figures of the preparation cellular tin dioxide material of gained in the embodiment of the present invention；
Fig. 4 is the TEM figures of the preparation cellular tin dioxide material of gained in the embodiment of the present invention；
Fig. 5 is to prepare the cellular tin dioxide material of gained in the embodiment of the present invention to experience of short duration laser burns on surface
Front and rear Raman test chart；
Fig. 6 is the thermogravimetric analysis figure of the preparation cellular tin dioxide material of gained in Example 1 and Example 2 of the present invention；
Fig. 7 is that the cellular tin dioxide material of gained is prepared in the embodiment of the present invention in lithium ion battery small current
(100mA g-1) discharge and recharge cycle performance figure；
Fig. 8 is that the cellular tin dioxide material of gained is prepared in the embodiment of the present invention in sodium-ion battery small current
(100mA g-1) discharge and recharge cycle performance figure.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only used to explain the present invention, not
For limiting the present invention.
Fig. 1 shows the preparation principle figure of the electrode material that present example is provided, and for convenience of description, illustrate only and this
The relevant portion of inventive embodiments step c, details are as follows：
Specific embodiment one：A kind of system of cellular tin ash lithium (sodium) ion battery cathode material of present embodiment
Preparation Method, realizes according to the following steps：
The preparation of silicon oxide pellets：61.75mL ethanol and 24.75mL deionized waters is measured to be stirred in same beaker
Well mixed, the mass fraction of the tetraethyl orthosilicate and 9mL that then add 4.5mL is 25% ammoniacal liquor, is stirred at room temperature
Mix 8 hours, be centrifuged and washed respectively repeatedly with deionized water and alcohol and be dried overnight at 60 DEG C and obtain product；
The preparation of tin ash coated silica bead：Weigh 0.04g silicon oxide pellets and ultrasonic disperse is in 60mL
Water and alcohol mixeding liquid in obtain white suspension, wherein the volume fraction of ethanol be 37.5%；0.3g is added afterwards
Three hydrated stannic acid potassium and 1.8g urea and after continuously stirring 5 minutes, suspension are transferred in the water heating kettle of 100mL, in 170 DEG C
Product is obtained after lower reaction 18 hours, centrifuge washing and drying；
The preparation of cellular tin ash/carbon composite electrode material：Tin ash prepared by previous step coats dioxy
SiClx bead takes that 0.2g ultrasonic disperses add 0.1g glucose in 67mL deionized waters, then and 10g sodium chloride is dissolved in
Wherein；Solution is heated to seethe with excitement and be stirred continuously make moisture evaporating completely after obtain white powder, be placed in tube furnace
Natural cooling after 650 DEG C and three hours of insulation is heated under the atmosphere of argon gas, gained black solid is dispersed in 2mol/L
Sodium hydroxide solution in and soak 8 hours, filtration washing drying repeatedly and at 60 DEG C obtains prepared novel electrode
Material.
Raw material and laboratory apparatus used in present embodiment are readily available, and implementation condition is easily realized.
Specific embodiment two：This specific embodiment from unlike specific embodiment one, in step cellular two
0.2g glucose and 10g sodium chloride are dissolved in dispersion liquid in the preparation of tin oxide/carbon composite electrode material.Other specification and
Specific implementation step is identical with specific embodiment one.This embodiment two is increased made using the carbon source usage amount of greater proportion
The ratio of carbon, is played a part of for carbon-coating in research institute's design structure in standby sample.
In the above embodiments step, under conditions of other steps and parameter keep constant, the cellular dioxy of step
The addition for changing organic matter in the preparation of tin/carbon composite electrode material is the key factor of Control release variable.
Two kinds of parameters are employed in embodiment, is respectively 0.1g glucose and 0.2g glucose.Difference between the two exists
The organic matter added in experimentation is that the ratio of carbon source is different, causes the carbon content in synthesized material different.By surveying
Examination show that the carbon content of resulting materials in embodiment one and embodiment two is respectively 28.6% and 43.6%, and different carbon contains
Amount causes corresponding influence to the performance of material really.The resulting materials of embodiment one contain lower carbon content, contain simultaneously
Active material tin ash content higher, so as to have bigger specific capacity relative to embodiment two.Embodiment one and two is equal
With similar carbon structure, there is identical advantage, material prepared by two embodiments in terms of the cyclical stability of material is ensured
Material is demonstrated by excellent cyclical stability.
The stannic oxide electrode material prepared using example one is in powdered, and being tested by XRD can determine sample
In comprise only tin ash and carbon, there is no the presence (see Fig. 2) of other impurities phase；And the microcosmic of material is drawn by electron microscopic observation
Pattern is coated on structure (see Fig. 3, Fig. 4) in the middle of ultrathin carbon films in similar to cellular hollow tin ash bead, and this is new
The structure of grain husk provides guarantee for the stability of electrode；By drawing of the contrast material before and after of short duration laser surface calcination is experienced
Graceful figure (see Fig. 5) can be seen that the Raman peaks to can just detect tin ash after the slight calcination of carbon of material surface, explanation
Tin ash is coated within carbon film；Embodiment one and sample is tested by thermogravimetric analysis respectively obtained in embodiment two
Go out wherein tin ash content it is different be respectively 71.4% and 56.4% (see Fig. 6), with the carbon source amount for adding number be consistent；
Electrode material obtained in embodiment one is circulated test as to electrode assembling with sodium piece using lithium piece into battery respectively, can obtain
It is 100mA g to go out the material in current density-1Lower lithium storage content and storage sodium capacity are respectively 928.9 and 251.5mAh g-1(ginseng
See Fig. 7, Fig. 8), it is seen that the material has good cyclical stability, and lithium storage content and storage sodium capacity higher, with certain
Some commercial potential.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, it is not used to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc., all should include
Within protection scope of the present invention.
Claims (5)
1. a kind of preparation method of cellular tin dioxide material, it is characterised in that the method comprises the following steps：
Step one：The preparation of silicon oxide pellets
Take 60-70mL ethanol and 30-40mL deionized waters are uniformly mixed in same beaker, add the positive silicon of 4-5mL
The mass fraction of sour tetra-ethyl ester and 8-10mL is 25% ammoniacal liquor, is stirred at room temperature 8-12 hours, is centrifuged and uses deionized water
Washed respectively with alcohol multiple and dried；
Step 2：The preparation of tin ash coated silica bead
Weigh 0.03-0.06g silicon oxide pellets and the ultrasonic disperse water and ethanol in 50-70mL of a kind of acquisition of the step
In mixed liquor, wherein the volume fraction of ethanol is 37.5-45%；The pink salt and 1.2- of 0.3-0.4g facile hydrolysis are added afterwards
1.8g urea and after continuously stirring 5-10 minutes, suspension is transferred in the water heating kettle of 100mL, in being reacted at 160-180 DEG C
12-18 hours, product is obtained after centrifuge washing and drying；
Step 3：The preparation of cellular tin dioxide material
Tin ash coated silica bead prepared by the step 2 is taken into 0.2-0.3g, ultrasonic disperse goes in 50-70mL
In ionized water, the water soluble salt dissolving of 0.1-0.3g organic solutes and 8-10g cubics is added wherein；It is heated to boiling
And be stirred continuously make moisture evaporating completely after obtain white powder, it is heated to 550-700 DEG C under the atmosphere of protective gas
And natural cooling after 2-3 hours is incubated, gains are dispersed in the NaOH of 2-3mol/L or hydrofluoric acid solution and soaked
8-12 hour, filtration washing repeatedly and is dried.
2. the preparation method of cellular tin dioxide material as claimed in claim 1, it is characterised in that the tin of the facile hydrolysis
Salt is the hydrate of three hydrated stannic acid potassium, stannic chloride or stannous chloride or above-mentioned material.
3. the preparation method of cellular tin dioxide material as claimed in claim 2, it is characterised in that the organic solute
It is glucose, sucrose or citric acid.
4. in a kind of 1-3 such as claim as described in any one prepared by the preparation method of cellular tin dioxide material two
Stannic oxide materials.
5. the material prepared by a kind of preparation method of the cellular tin dioxide material in 1-4 such as claim as described in any one
Material produced lithium or anode material of lithium-ion battery.
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| CN110092414A (en) * | 2018-01-30 | 2019-08-06 | 北京大学 | One kind has the metal oxide materials and preparation method thereof of special microstructure |
| CN113233497A (en) * | 2021-05-18 | 2021-08-10 | 哈尔滨工业大学 | Preparation method and application of carbon-coated tin dioxide material |
| CN114988419A (en) * | 2022-05-25 | 2022-09-02 | 陕西科技大学 | SiO (silicon dioxide) 2 SnSe/C nanosphere and preparation method thereof |
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| CN110092414B (en) * | 2018-01-30 | 2021-01-26 | 北京大学 | Metal oxide material with special microstructure and preparation method thereof |
| CN113233497A (en) * | 2021-05-18 | 2021-08-10 | 哈尔滨工业大学 | Preparation method and application of carbon-coated tin dioxide material |
| CN114988419A (en) * | 2022-05-25 | 2022-09-02 | 陕西科技大学 | SiO (silicon dioxide) 2 SnSe/C nanosphere and preparation method thereof |
| CN114988419B (en) * | 2022-05-25 | 2023-12-08 | 陕西科技大学 | SiO (silicon dioxide) 2 SnSe/C nanospheres and preparation method thereof |
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