CN110098391A - Titanium dioxide/carbon-coated nano silicon trielement composite material derived from a kind of MXene and preparation method thereof - Google Patents
Titanium dioxide/carbon-coated nano silicon trielement composite material derived from a kind of MXene and preparation method thereof Download PDFInfo
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- CN110098391A CN110098391A CN201910314754.7A CN201910314754A CN110098391A CN 110098391 A CN110098391 A CN 110098391A CN 201910314754 A CN201910314754 A CN 201910314754A CN 110098391 A CN110098391 A CN 110098391A
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The present invention provides titanium dioxide derived from a kind of MXene/carbon-coated nano silicon trielement composite materials and preparation method thereof.Negatively charged MXene is coated on positively charged nanometer silicon face by electrostatic self-assembled method, MXene is then oxidized to TiO in air atmosphere2/ C forms TiO2The trielement composite material of/C cladding nano-silicon.Wherein, MXene Ti3C2Tx、Ti2CTxOne or both of；The size of nano-silicon is 50-500 nm;The mass ratio of MXene and nano-silicon is 1:1-4；MXene oxidizing temperature is 200-300 DEG C, and titanium dioxide/carbon-coating is with a thickness of 2-10nm.Titanium dioxide/carbon is in nano-silicon coated with uniform in titanium dioxide derived from MXene of the invention/carbon-coated nano silicon trielement composite material, regular appearance, preparation method is simple, cost is relatively low, it can be prepared on a large scale, there is excellent cycle performance and high rate performance for lithium ion battery negative material.
Description
Technical field
The present invention relates to a kind of titanium dioxide derived from MXene/carbon-coated nano silicon trielement composite material and its preparation sides
Method.
Background technique
As the development and people of economic society are for the growing of energy demand, lithium ion battery is due to its high energy
Metric density, long circulation life, memory-less effect and it is highly-safe the features such as gradually show one's talent in numerous energy storage devices,
It is widely used in the fields such as portable electronic device, electric car and aerospace.However at present commercialized lithium from
Sub- battery is not able to satisfy requirement of the people for high-energy density and high power density in aspect of performance, therefore finds a new generation
The electrode material of high capacity is extremely urgent.
In numerous negative electrode materials of lithium ion battery, the theoretical specific capacity of silicon materials is up to 4200 mAh g-1, it is tradition
10 times or more of graphite cathode, therefore silica-base material is applied to lithium ion battery negative material as research hotspot.But silicon
Huge volume expansion and low conductivity are shown during intercalation/deintercalation lithium as negative electrode material, are seriously affected
The cycle performance and high rate performance of battery, cause it not to be able to satisfy the needs of practical application.It, can by the sized nanostructures of silicon materials
To be effectively improved the chemical property of silicon materials.On the other hand, the structure of silicon materials is regulated and controled, such as porous structure, nucleocapsid
Structure etc. can effectively buffer volume expansion of the silicon in battery charge and discharge process.Core-shell structure is as most commonly seen regulation
The mode of silica-base material structure, can not only improve the electric conductivity of electrode, and can be avoided the direct contact of silicon and electrolyte,
SEI layers of uncontrollable growth is reduced, and then largely improves the cyclical stability of electrode.In numerous surface coating layer materials
In material, coating of titanium dioxide one side elasticity with higher can buffer volume expansion of the silicon in battery charge and discharge process；
On the other hand, titanium dioxide has excellent thermal stability, can inhibit fever phenomenon of the silicon in charge and discharge process, therefore draw
The extensive concern of people is played.However, coating of titanium dioxide electric conductivity is poor, not can effectively improve after being coated to silicon materials
The electric conductivity of material.
Transition metal carbide or nitride, also referred to as MXene are the New Two Dimensional materials found for the first time for 2011, it
Have the characteristics that the high conductivity of graphene and graphene oxide are hydrophilic, minimum nanometer thickness flexibly adjustable but also with component
The advantages such as controllable, present huge potentiality in the application aspect of secondary cell and the electrode material of supercapacitor.Meanwhile
MXene is easily aoxidized in air, is changed into the compound of oxide and carbon.
Since coating of titanium dioxide is not enough to improve conductivity of composite material, introduce carbon material construct three-dimensional composite material with
The electric conductivity for improving composite material becomes effective way.However, how to regulate and control titanium dioxide, carbon, silicon three structure, make compound
Material has excellent chemical property, is still a challenging problem.
Summary of the invention
In view of the problems of the existing technology, the purpose of the present invention is to provide titanium dioxide/carbon derived from a kind of MXene
Nano-silicon trielement composite material and preparation method thereof is coated, titanium dioxide derived from the MXene/carbon-coated nano silicon ternary is multiple
Condensation material is after negatively charged MXene is evenly coated at positively charged nanometer silicon face by electrostatic self-assembled method, in sky
MXene is oxidized to titanium dioxide/carbon and is formed by high temperature under gas atmosphere.Wherein, coating of titanium dioxide is uniform in nanometer silicon face
Cladding, can effectively buffer volume expansion of the nano-silicon in charge and discharge process, the uniform carbon material of coating surface can be effective
Improve the electric conductivity of trielement composite material, and then improves the chemical property of composite material.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of titanium dioxide/carbon-coated nano silicon trielement composite material derived from MXene, which is characterized in that the MXene
Derivative titanium dioxide/carbon-coated nano silicon trielement composite material is negatively charged MXene uniform by electrostatic self-assembled method
It is coated on after positively charged nanometer silicon face high temperature in air atmosphere MXene is oxidized to titanium dioxide/carbon and formed；
The MXene is Ti3C2Tx、Ti2CTxOne or both of；
The size of the nano-silicon is 50-500 nm；
The mass ratio of the MXene and positively charged nano-silicon is 1:1-4；
The MXene oxidizing temperature is 200-300 DEG C；
Titanium dioxide/the layer with a thickness of 2-10nm.
Wherein, titanium dioxide derived from the MXene/carbon-coated nano silicon trielement composite material is prepared by the following method
It obtains:
(1) 1g nano-silicon, 5 ml 3-aminopropyltriethoxysilane (APTES) and 150 ml dehydrated alcohols are added to
In three-necked flask, 110 DEG C of 6 h of reflux carry out amination processing to nano-silicon, keep nanometer silicon face positively charged；
(2) using MAX phase material as raw material, by etching and removing preparation MXene aqueous solution
(3) positively charged nano-silicon is added in the resulting MXene solution of step (2) by certain mass ratio, stirring is certain
It is filtered after time and obtains MXene cladding nanometer silicon composite material；
(4) the MXene cladding nanometer silicon composite material that step (3) obtains is heated in air atmosphere and is obtained derived from MXene
Titanium dioxide/carbon-coated nano silicon trielement composite material.
Optionally, MAX phase material described in step (2) is Ti3AlC2、Ti2One or both of AlC；
Optionally, step (2) the MXene solution preparation the following steps are included:
A, 0.99g LiF is added in the plastic bottle equipped with 10ml hydrochloric acid, stirs 5min, adds 1 g MAX phase material, stir
It mixes uniformly；
B, the mixed liquor for obtaining step A is placed in 35 DEG C of thermostat water baths, is stirred to react for 24 hours；
C, the solution that step B is obtained is centrifuged plus water operates 4 times repeatedly, until pH value of solution ≈ 6, goes supernatant liquor, ultrasound 30
Min is centrifuged 1h, collects upper solution, the MXene solution after being etched.
Optionally, mass ratio described in step (3) is MXene: positively charged nano-silicon=1:1-4；
Optionally, mixing time described in step (3) is 0.5-2h；
Optionally, heated oxide temperature described in step (4) is 200-300 DEG C.
Compared with prior art, this method has the advantage that
1, the present invention provides a kind of titanium dioxide derived from MXene/carbon-coated nano silicon trielement composite material preparation method,
The negatively charged MXene in surface can be uniformly coated on the surface of nano-silicon by electrostatic self-assembled method, it is oxidation-treated can
On the surface of nano-silicon, the one step compound in situ for directly forming titanium dioxide and carbon, titanium dioxide/carbon complex are highly uniform
Ground is coated on the surface of nano-silicon；
2, the present invention provides a kind of titanium dioxide derived from MXene/carbon-coated nano silicon trielement composite material preparation method,
Titanium dioxide elastic coating can effectively buffer nano-silicon in charge and discharge in the titanium dioxide/carbon-coating formed after MXene oxidation processes
Volume expansion in electric process, and the carbon on coating of titanium dioxide surface can effectively improve the electric conductivity of composite material, Jin Erti
The chemical property of high composite material；
3, the present invention provides a kind of titanium dioxide derived from MXene/carbon-coated nano silicon trielement composite material preparation method,
The trielement composite material pattern of this method preparation is good, and the mass ratio of titanium dioxide/carbon and nano silicon material can pass through
The quality of MXene and nano-silicon is adjusted easily to regulate and control；
4, the present invention provides a kind of titanium dioxide derived from MXene/carbon-coated nano silicon trielement composite material preparation method,
This method reaction yield is high, is suitable for being mass produced.
Detailed description of the invention
Fig. 1 is titanium dioxide/carbon-coated nano silicon trielement composite material derived from the MXene of the preparation of the embodiment of the present invention 1
Scanning electron microscope (SEM) figure.
Fig. 2 is titanium dioxide/carbon-coated nano silicon trielement composite material derived from the MXene of the preparation of the embodiment of the present invention 1
Cycle performance curve graph as lithium ion battery negative material.
Fig. 3 is titanium dioxide/carbon-coated nano silicon trielement composite material derived from the MXene of the preparation of the embodiment of the present invention 2
Transmission electron microscope (TEM) figure.
Fig. 4 is titanium dioxide/carbon-coated nano silicon trielement composite material derived from the MXene of the preparation of the embodiment of the present invention 3
As lithium ion battery negative material cycle performance figure.
Specific embodiment
Further clear and complete explanation is done to technical solution provided by the invention below by the mode of specific embodiment,
But they are not construed as limiting the invention.
Embodiment 1
(1) modification of nanometer silicon face
1g nano-silicon, 5 ml 3-aminopropyltriethoxysilane (APTES) and 150 ml dehydrated alcohols are added to three mouthfuls
In flask, 110 DEG C of 6 h of reflux carry out amination processing to nano-silicon, keep nanometer silicon face positively charged.
(2) synthesis of MXene
0.99g LiF is added in the plastic bottle equipped with 10ml hydrochloric acid, 5min is stirred, dissolves LiF, add 1 g
Ti2AlC is stirred evenly.Obtained mixed liquor is placed in 35 DEG C of thermostat water baths, stirring etching is for 24 hours.It will be upper after etching reaction
Stating product adds water, centrifugation to operate 4 times repeatedly, until supernatant liquor pH ≈ 6, removes supernatant liquor, again plus water, ultrasonic 30min, from
Heart 1h, collects upper solution, and the MXene solution after being etched measures 5ml MXene solution and filters, weighs after drying, obtains
MXene concentration is 2.9mg/ml.
(3) titanium dioxide derived from MXene/carbon-coated nano silicon trielement composite material preparation
The positively charged nano-silicon of 200mg is added in 200ml deionized water, ultrasonic 20min keeps its evenly dispersed.To above-mentioned
68.97ml MXene aqueous solution (200mg) is added in dispersion liquid, stirs 0.5h, is collected by centrifugation, it is dry, obtain MXene cladding
Nanometer silicon composite material.Above-mentioned material is placed in 200 DEG C of heat treatment 2h in Muffle furnace, obtain titanium dioxide derived from MXene/
Carbon-coated nano silicon trielement composite material.
(4) material characterization and performance of lithium ion battery test
Titanium dioxide derived from MXene/carbon-coated nano silicon trielement composite material is subjected to characterization test.SEM(Fig. 1) show by
After the processing of MXene heated oxide, titanium dioxide/carbon-coating can be evenly coated at a nanometer silicon face.By above-mentioned material according to active matter
Matter: acetylene black: the ratio of CMC=80:10:10 be mixed with electrode slice as cathode, polypropylene porous film (Celgard
3501) diaphragm, electrolyte are 1mol/L LiPF6/ EC/DEC(V:V=1:1) mixed solution.Battery is being full of high-purity argon gas
It is assembled in glove box.Constant current charge-discharge test (voltage range 0.01-2.5V) shows in 500 mAh g-1Current density
After lower circulation 100 times, battery capacity is up to 456.2mAh g-1(Fig. 2) is significantly better than the cycle performance of pure silicon material.
Embodiment 2
(1) modification of nanometer silicon face
1g nano-silicon, 5 ml 3-aminopropyltriethoxysilane (APTES) and 150 ml dehydrated alcohols are added to three mouthfuls
In flask, 110 DEG C of 6 h of reflux carry out amination processing to nano-silicon, keep nanometer silicon face positively charged.
(2) synthesis of MXene
0.99g LiF is added in the plastic bottle equipped with 10ml hydrochloric acid, 5min is stirred, dissolves LiF, add 1 g
Ti2AlC is stirred evenly.Obtained mixed liquor is placed in 35 DEG C of thermostat water baths, stirring etching is for 24 hours.It will be upper after etching reaction
Stating product adds water, centrifugation to operate 4 times repeatedly, until supernatant liquor pH ≈ 6, removes supernatant liquor, again plus water, ultrasonic 30min, from
Heart 1h, collects upper solution, and the MXene solution after being etched measures 5ml MXene solution and filters, weighs after drying, obtains
MXene concentration is 2.9mg/ml.
(3) titanium dioxide derived from MXene/carbon-coated nano silicon trielement composite material preparation
The positively charged nano-silicon of 200mg is added in 200ml deionized water, ultrasonic 20min keeps its evenly dispersed.To above-mentioned
17.24ml MXene aqueous solution (50mg) is added in dispersion liquid, stirs 1h, is collected by centrifugation, it is dry, obtain MXene cladding nanometer
Silicon composite.Above-mentioned material is placed in 300 DEG C of heat treatment 2h in Muffle furnace, obtains titanium dioxide derived from MXene/carbon packet
Cover nano-silicon trielement composite material.
(4) material characterization and performance of lithium ion battery test
Titanium dioxide derived from MXene/carbon-coated nano silicon trielement composite material is subjected to characterization test.TEM(Fig. 3) show two
Titanium oxide/carbon-coating can be evenly coated at a nanometer silicon face, and thickness is about 5nm.By above-mentioned material according to active material: acetylene black:
The ratio of CMC=80:10:10 be mixed with electrode slice as cathode, polypropylene porous film (Celgard 3501) diaphragm,
Electrolyte is 1mol/L LiPF6/ EC/DEC(V:V=1:1) mixed solution.Battery full of high-purity argon gas glove box in into
Row assembling.Constant current charge-discharge test (voltage range 0.01-2.5V) shows in 500 mAh g-1Current density under recycle 100
After secondary, battery capacity is up to 856.2mAh g-1, show excellent cycle performance.
Embodiment 3
(1) modification of nanometer silicon face
1g nano-silicon, 5 ml 3-aminopropyltriethoxysilane (APTES) and 150 ml dehydrated alcohols are added to three mouthfuls
In flask, 110 DEG C of 6 h of reflux carry out amination processing to nano-silicon, keep nanometer silicon face positively charged.
(2) synthesis of MXene
0.99g LiF is added in the plastic bottle equipped with 10ml hydrochloric acid, 5min is stirred, dissolves LiF, add 1g
Ti3AlC2, stir evenly.Obtained mixed liquor is placed in 35 DEG C of thermostat water baths, stirring etching is for 24 hours.It will be upper after etching reaction
Stating product adds water, centrifugation to operate 4 times repeatedly, until supernatant liquor pH ≈ 6, removes supernatant liquor, again plus water, ultrasonic 30min, from
Heart 1h, collects upper solution, and the MXene solution after being etched measures 5ml MXene solution and filters, weighs after drying, obtains
MXene concentration is 2.0mg/ml.
(3) titanium dioxide derived from MXene/carbon-coated nano silicon trielement composite material preparation
The positively charged nano-silicon of 200mg is added in 200ml deionized water, ultrasonic 20min keeps its evenly dispersed.To above-mentioned
200ml MXene aqueous solution (400mg) is added in dispersion liquid, stirs 0.5h, is collected by centrifugation, it is dry, it obtains MXene cladding and receives
Rice silicon composite.Above-mentioned material is placed in 200 DEG C of heat treatment 2h in Muffle furnace, obtains titanium dioxide/carbon derived from MXene
Coat nano-silicon trielement composite material.
(4) performance of lithium ion battery is tested
Using above-mentioned material according to active material: acetylene black: the ratio of CMC=80:10:10 be mixed with electrode slice as negative
Pole, polypropylene porous film (Celgard 3501) diaphragm, electrolyte are 1mol/L LiPF6/ EC/DEC(V:V=1:1) mixing
Solution.Battery is assembled in the glove box full of high-purity argon gas.Constant current charge-discharge test (voltage range 0.01-2.5V) table
It is bright, in 500 mAh g-1Current density under recycle 400 times after, battery capacity is up to 529.6mAh g-1(Fig. 4), shows
Excellent cycle performance.
Claims (7)
1. titanium dioxide derived from a kind of MXene/carbon-coated nano silicon trielement composite material and preparation method thereof, feature exists
In titanium dioxide derived from the MXene/carbon-coated nano silicon trielement composite material is that negatively charged MXene passes through electrostatic
Self-assembly method is coated on positively charged nanometer silicon face, and MXene is then oxidized to titanium dioxide/carbon in air atmosphere again
Clad is formed；
The MXene is Ti3C2Tx、Ti2CTxOne or both of；
The size of the nano-silicon is 50-500 nm；
The mass ratio of the MXene and positively charged nano-silicon is 1:1-4；
The MXene oxidizing temperature is 200-300 DEG C；
Titanium dioxide/the layer with a thickness of 2-10nm.
2. titanium dioxide derived from MXene described in a kind of claim 1/carbon-coated nano silicon trielement composite material and its preparation side
Method, which comprises the steps of:
(1) 1g nano-silicon, 5 ml 3-aminopropyltriethoxysilane (APTES) and 150 ml dehydrated alcohols are added to
In three-necked flask, 110 DEG C of 6 h of reflux carry out amination processing to nano-silicon, keep nanometer silicon face positively charged；
(2) using MAX phase material as raw material, by etching and removing preparation MXene aqueous solution
(3) positively charged nano-silicon is added in the resulting MXene solution of step (2) according to certain mass ratio, stirring one
It is filtered after fixing time and obtains MXene cladding nanometer silicon composite material；
(4) heating the MXene cladding nanometer silicon composite material that step (3) obtains in air atmosphere makes MXene aoxidize to obtain
Titanium dioxide derived from MXene/carbon-coated nano silicon trielement composite material.
3. titanium dioxide derived from a kind of MXene according to claim 2/carbon-coated nano silicon trielement composite material system
Preparation Method, which is characterized in that MAX phase material described in step (2) is Ti3AlC2、Ti2One or both of AlC.
4. titanium dioxide derived from a kind of MXene according to claim 2/carbon-coated nano silicon trielement composite material system
Preparation Method, which is characterized in that the preparation of step (2) the MXene solution the following steps are included:
A, 0.99g LiF is added in the plastic bottle equipped with 10ml hydrochloric acid, stirs 5min, adds 1 g MAX phase material, stir
It mixes uniformly；
B, the mixed liquor for obtaining step A is placed in 35 DEG C of thermostat water baths, is stirred to react for 24 hours；
C, the solution that step B is obtained is centrifuged plus water operates 4 times repeatedly, until pH value of solution ≈ 6, goes supernatant liquor, ultrasound 30
Min is centrifuged 1h, collects upper solution, obtains MXene solution.
5. titanium dioxide derived from a kind of MXene according to claim 2/carbon-coated nano silicon trielement composite material system
Preparation Method, which is characterized in that certain mass ratio described in step (3) is MXene: positively charged nano-silicon=1:1-4.
6. titanium dioxide derived from a kind of MXene according to claim 2/carbon-coated nano silicon trielement composite material system
Preparation Method, which is characterized in that mixing time described in step (3) is 0.5-2h.
7. a kind of preparation method of MXene/ nitrogen-doped carbon combination electrode material according to claim 2, which is characterized in that
Heated oxide temperature described in step (4) is 200-300.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111384381A (en) * | 2020-03-23 | 2020-07-07 | 北京化工大学 | Silicon @ carbon/MXene ternary composite material for lithium ion battery and preparation method thereof |
| CN112103504A (en) * | 2020-09-22 | 2020-12-18 | 广东工业大学 | Ternary material loaded few-layer/rod-shaped MXene composite material and preparation method thereof |
| CN113066965A (en) * | 2021-03-22 | 2021-07-02 | 宁波杉杉新材料科技有限公司 | MXene-silicon composite anode material, battery containing MXene-silicon composite anode material, and preparation method and application of MXene-silicon composite anode material |
| CN114388760A (en) * | 2022-01-14 | 2022-04-22 | 北京化工大学 | Metal oxide nanosheet material, preparation method thereof and lithium ion battery |
| CN114512640A (en) * | 2020-11-16 | 2022-05-17 | 哈尔滨工程大学 | Sulfur-based positive electrode material of all-solid-state battery and preparation method thereof |
| CN114538505A (en) * | 2022-03-18 | 2022-05-27 | 中国地质大学（武汉） | Nano flaky TiS2/Ti3C2TX MXene/C composite material and preparation method and application thereof |
| CN115020680A (en) * | 2022-07-15 | 2022-09-06 | 山东大学 | MXene-coated hard carbon negative electrode material of sodium ion battery |
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