CN105470486A - Preparation method of granular tin dioxide/two-dimensional nano titanium carbide composite material - Google Patents

Preparation method of granular tin dioxide/two-dimensional nano titanium carbide composite material Download PDF

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CN105470486A
CN105470486A CN201510991800.9A CN201510991800A CN105470486A CN 105470486 A CN105470486 A CN 105470486A CN 201510991800 A CN201510991800 A CN 201510991800A CN 105470486 A CN105470486 A CN 105470486A
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mxene
composite material
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CN105470486B (en
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王芬
王子婧
曹敏娟
朱建锋
杨海波
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Shaanxi University of Science and Technology
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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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/46—Metal oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • 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

Abstract

The invention provides a preparation method of a tin dioxide/two-dimensional nano titanium carbide composite material. The preparation method comprises: carrying out ball milling on ternary layered Ti3AlC2 ceramic powder; immersing the obtained product in hydrofluoric acid solution to perform the reaction for 6h to 120h; stirring, centrifugally cleaning a corrosion product by using deionized water, and drying an obtained solid sample to obtain a two-dimensional layered nano material MXene-Ti3C2; and mixing SnCl4.5H2O, glucose and the two-dimensional nano MXene-Ti3C2, using ethanol as a solvent, adjusting PH to 12 to 14, stirring with a magnetic force for 2h, performing the reaction at 120 DEG C for 6h, and after naturally cooling to a room temperature, carrying out centrifuging and drying to obtain a SnO2/MXene-Ti3C2 composite material. The material obtained by the preparation method can effectively alleviate a volume effect of SnO2 nano particles, and the SnO2/MXene-Ti3C2 nano composite material has an excellent application prospect in the field of an anode material field of a high storage germanium lithium ion battery.

Description

The preparation method of graininess tin ash/two-dimensional nano titanium carbide composite material
Technical field
The invention belongs to nano-functional material preparation and applied technical field thereof, be specifically related to the preparation method of graininess tin ash/two-dimensional nano titanium carbide composite material.
Background technology
Two-dimensional layer nano-carbide MXene-Ti 3c 2it is the material of a kind graphene-structured, ultra-thin two-dimension nanometer sheet has superpower catalytic performance, photovoltaic performance and chemical property due to the synusia thickness of the appearance structure of its uniqueness, less particle size, larger surface volume ratio and atom level, be widely used in functional ceramic, photocatalysis, lithium ion battery, solar cell, gas sensor etc., but two-dimensional layer nano-carbide MXene-Ti 3c 2not easily directly synthesize, and by Ti 3alC 2ceramic powder is prepared as predecessor, becomes a kind of simple method.
Ternary layered Ti 3alC 2material has special crystal structure, is typical strong covalent bond between Ti and C, and Al atomic layer is inner and be weak metallic bond between Al atom and Ti, and the process that is easy to be corroded of Al wherein removes and obtains the Ti of two-dimensional layer class graphene-structured 3c 2,metal oxide-loaded on this, then can realize the compound of material several functions and structure.
The oxide of tin receives much attention because of having height ratio capacity and low embedding lithium electromotive force, once the most promising sub of carbon negative pole material was considered to, but also there are some shortcomings in it, if volumetric expansion in first charge-discharge process is up to more than 50%, the cycle period embedding repeatedly of lithium ion easily occurs with deviating from process " efflorescence " with " reunion " phenomenon, these all cause the oxide electrochemical performance of tin to decline rapidly, thus limit its extensive use in lithium ion battery.
The people such as Ma Weike prepare graphene-based stannic oxide nanometer composite material and have studied its chemical property, and experimental result shows that graphene-based tin ash significantly improves (Ma Weike .SnO as the charge/discharge capacity of lithium ion battery negative material 2/ graphene composite material Electrochemical Properties [D]. the Yanshan Mountain: University On The Mountain Of Swallows, 2011.); The people such as Zhu adopt hydro thermal method to prepare SnO 2/ graphite nano composite material also shows that its performance in lithium ion battery, photocatalysis etc. is all better than single grapheme material (YunGuangZhu, YeWang, JianXie, Gao-ShaoCao, Tie-JunZhu, XinbingZhao, HuiYingYang, EffectsofGrapheneOxideFunctionGroupsonSnO 2/ GrapheneNanocompositesforLithiumStorageApplication, [J] .ElectrochimicaActa.154 (2015) 338 – 344.). but above-mentioned research is all by SnO 2load is on Graphene, and Graphene effectively can not alleviate SnO 2bulk effect, and at Li +easily damage in deintercalation process.The present invention selects MXene-Ti 3c 2two-dimensional layer material load SnO 2, be wherein typical strong covalent bond between Ti and C, effectively can alleviate SnO 2the phenomenon such as efflorescence reunion.Improve above shortcoming, tin ash/two-dimensional layer nano titanium carbide (MXene) composite material can be made, be expected to there is good application in fields such as photocatalysis, waste water treatment, lithium ion battery, ultracapacitor, biology sensors.
Summary of the invention
In order to overcome the defect of above-mentioned prior art, the object of the present invention is to provide the preparation method of graininess tin ash/two-dimensional nano titanium carbide composite material, by hydro-thermal reaction by SnCl 45H 2o generates SnO under alkaline environment 2load to MXene-Ti 3c 2nano-material surface, thus the preparation method that a kind of graininess tin ash/two-dimensional nano titanium carbide (MXene) composite material is provided; First will synthesize and Ti after processing 3alC 2powder carries out chemical etching in HF acid, and Al is etched away by selectivity, forms a kind of two-dimensional layer material MXene-Ti 3c 2, then at two-dimensional layer material MXene-Ti 3c 2upper load SnO 2, make MXene-Ti 3c 2specific surface larger, taken into account SnO 2advantage, as photocatalysis performance, one's own physical property, pattern is various.
In order to achieve the above object, technical scheme of the present invention is as follows:
The preparation method of graininess tin ash/two-dimensional nano titanium carbide composite material, is characterized in that, comprise the steps:
(1) ternary layered Ti is first prepared according to the method for patent ZL201310497696.9 3alC 2ceramic powder, then by powder high-energy ball milling 1h-4h, rotating speed 400r/min, ratio of grinding media to material 10:1,40 DEG C-60 DEG C oven dry after refinement powder, obtain particle diameter at the Ti of 8 μm-75 μm 3alC 2ceramic powder;
(2) by gained Ti in step (1) 3alC 2ceramic powder gets 2g ~ 10g under 60 DEG C of conditions, is immersed in 50mL ~ 200mL35wt% ~ 45wt% hydrofluoric acid solution and reacts 6h ~ 120h; Stir, corrosion product is used deionized water eccentric cleaning, until centrifuged supernatant pH is between 5 ~ 6; Then washes of absolute alcohol is used 2 ~ 4 times; Gained solid sample is dry, obtain two-dimensional layer nano material MXene-Ti 3c 2;
(3) by SnCl 45H 2o, glucose and step (2) gained two-dimensional nano MXene-Ti 3c 2mixing, Sn 4+be 3:1, SnCl with the mol ratio of glucose 45H 2o and two-dimensional nano MXene-Ti 3c 2mass ratio is 2:1, using ethanol as solvent, uses NH 3h 2o regulates PH to 12-14, uses magnetic agitation 2h, mixed liquor is added polytetrafluoroethylene reactor and reacts 120 DEG C, 6h, and after naturally cooling to room temperature, centrifugal 20min washes 3 times, dries 12h for 50 DEG C subsequently, can obtain SnO 2/ MXene-Ti 3c 2composite material.
Advantage of the present invention is to utilize a step hydro-thermal reaction, makes SnO 2uniform load is at MXene-Ti 3c 2on, prepare the SnO that pattern is various 2/ MXene-Ti 3c 2composite material.And SnO 2/ MXene-Ti 3c 2composite material has excellent chemical property, and during as lithium ion battery negative material, discharge capacity can up to 1030mAhg first for it -1, make two-dimensional layer nano material MXene-Ti 3c 2open a new situation in the application aspect of lithium ion battery, its good thermal conductivity and electric conductivity have played huge effect.
The present invention selects MXene-Ti 3c 2two-dimensional layer material load SnO 2, be wherein typical strong covalent bond between Ti and C, effectively can alleviate SnO 2the phenomenon such as efflorescence reunion.Effectively improve capacitance, make its first charge-discharge capacity up to 1030.1mAhg -1.All improve significantly compared to the work of forefathers, tin ash/two-dimensional layer nano titanium carbide (MXene) composite material can be made, be expected to there is better application in the field such as lithium ion battery, ultracapacitor.
Accompanying drawing explanation
Fig. 1 is Ti 3alC 2after powder corrosion treatment, and corrosion product MXene-Ti 3c 2load SnO 2the XRD collection of illustrative plates of sample.
Fig. 2 (a) is Ti 3alC 2the SEM figure of powder granule, Fig. 2 (b) is MXene-Ti after corrosion treatment 3c 2sEM figure, Fig. 2 (c) is SnO 2/ MXene-Ti 3c 2the SEM figure of nano composite material, Fig. 2 (d) is SnO 2/ MXene-Ti 3c 2nano composite material local high power SEM scheme.
Embodiment
Further describe the present invention below by way of specific embodiments, the present invention also describes by other the scheme not departing from the technology of the present invention feature, and the change therefore within the scope of the present invention all or equivalent scope of the invention is all included in the invention.
Embodiment one
The present embodiment comprises the following steps:
(1) method of vacuum-sintering is adopted to prepare highly purified ternary layered Ti 3alC 2ceramic powder, then high-energy ball milling powder 4h, rotating speed 400r/min, ratio of grinding media to material 10:1,60 DEG C of oven dry after refinement powder.From Fig. 2 (a), SEM figure shows Ti 3alC 2the microscopic appearance of crystal, can find out that its grain size is about 8 μm, and obvious layer structure;
(2) by gained powder 2g in step (1) under 60 DEG C of conditions, be immersed in 100mL40% hydrofluoric acid solution and react 48h, stir, corrosion product is used deionized water eccentric cleaning, until centrifuged supernatant pH=5; Then washes of absolute alcohol is used 3 times; By gained solid sample drying at room temperature, obtain two-dimensional layer nano material MXene-Ti 3c 2, see Fig. 2 (b), wherein SEM figure shows MXene-Ti 3c 2microscopic appearance, can find out that its lamellar spacing is about 50nm, be typical two-dimensional layer nano material;
(3) hydro-thermal reaction, makes Sn 4+be 3:1 with the mol ratio of glucose, by SnCl 45H 2o and step (2) gained two-dimensional nano MXene-Ti 3c 2mix with the mass ratio of 2:1, using ethanol as solvent, use NH 3h 2o regulates PH to 12-14, uses magnetic agitation 2h, mixed liquor is added polytetrafluoroethylene reactor and reacts 120 DEG C, 6h, and after naturally cooling to room temperature, centrifugal 20min washes 3 times, dries 12h for 50 DEG C subsequently, can obtain SnO 2/ MXene-Ti 3c 2composite material.Visible SnO from Fig. 1 XRD collection of illustrative plates 2-Ti 3c 2containing SnO in powder 2and Ti 3c 2composition.See Fig. 2 (c) and (d), wherein SEM figure shows SnO 2/ MXene-Ti 3c 2the microscopic appearance of composite material, can find out SnO 2size is about 25nm, and is evenly distributed, and loads to MXene-Ti well 3c 2in two-dimensional layer nano material, form novel SnO 2/ MXene-Ti 3c 2nano composite material.
Embodiment two:
The present embodiment comprises the following steps:
(1) method of vacuum-sintering is adopted to prepare highly purified ternary layered Ti 3alC 2ceramic powder, then high-energy ball milling powder 1h, rotating speed 400r/min, ratio of grinding media to material 10:1, after refinement powder, 40 DEG C of oven dry, obtain Ti 3alC 2ceramic powder;
(2) by gained powder 2g in step (1) under the condition of 60 DEG C, be immersed in 50mL35% hydrofluoric acid solution and react 6h, stir, washed with de-ionized water is about 5 ~ 6 to pH, washes of absolute alcohol 2 times, centrifugation, gained solid sample is dry, obtain two-dimensional layer MXene-Ti 3c 2nano material;
(3) by SnCl 45H 2o, glucose and step (2) gained two-dimensional nano MXene-Ti 3c 2mixing, Sn 4+be 3:1, SnCl with the mol ratio of glucose 45H 2o and two-dimensional nano MXene-Ti 3c 2mass ratio, with 2:1, using ethanol as solvent, uses NH 3h 2o regulates PH to 12-14, uses magnetic agitation 2h, mixed liquor is added polytetrafluoroethylene reactor and reacts 120 DEG C, 6h, and after naturally cooling to room temperature, centrifugal 20min washes 3 times, dries 12h for 50 DEG C subsequently, can obtain SnO 2/ MXene-Ti 3c 2composite material.
Embodiment three
The present embodiment comprises the following steps:
(1) method of vacuum-sintering is adopted to prepare highly purified ternary layered Ti 3alC 2ceramic powder, then high-energy ball milling powder 3h, rotating speed 400r/min, ratio of grinding media to material 10:1,50 DEG C of oven dry after refinement powder;
(2) by gained powder 3g in step (1) under the condition of 60 DEG C, be immersed in 70mL35% hydrofluoric acid solution and react 24h, stir, corrosion product is used deionized water eccentric cleaning, until centrifuged supernatant pH is between 5 ~ 6; Then washes of absolute alcohol is used 3 times; Gained solid sample is dry, obtain two-dimensional layer nano material MXene-Ti 3c 2;
(3) by SnCl 45H 2o, glucose and step (2) gained two-dimensional nano MXene-Ti 3c 2mixing, Sn 4+be 3:1, SnCl with the mol ratio of glucose 45H 2o and two-dimensional nano MXene-Ti 3c 2mass ratio, with 2:1, using ethanol as solvent, uses NH 3h 2o regulates PH to 12-14, uses magnetic agitation 2h, mixed liquor is added polytetrafluoroethylene reactor and reacts 120 DEG C, 6h, and after naturally cooling to room temperature, centrifugal 20min washes 3 times,
Dry 12h for 50 DEG C subsequently, can SnO be obtained 2/ MXene-Ti 3c 2composite material.
Embodiment four
The present embodiment comprises the following steps:
(1) method of vacuum-sintering is adopted to prepare highly purified ternary layered Ti 3alC 2ceramic powder, then high-energy ball milling powder 3h, rotating speed 400r/min, ratio of grinding media to material 10:1,50 DEG C of oven dry after refinement powder;
(2) by gained powder 4g in step (1) under the condition of 60 DEG C, be immersed in 90mL40% hydrofluoric acid solution and react 48h, stir, corrosion product is used deionized water eccentric cleaning, until centrifuged supernatant pH is between 5 ~ 6; Then washes of absolute alcohol is used 4 times; Gained solid sample is dry, obtain two-dimensional layer nano material MXene-Ti 3c 2;
(3) by SnCl 45H 2o, glucose and step (2) gained two-dimensional nano MXene-Ti 3c 2mixing, Sn 4+be 3:1, SnCl with the mol ratio of glucose 45H 2o and two-dimensional nano MXene-Ti 3c 2mass ratio, with 2:1, using ethanol as solvent, uses NH 3h 2o regulates PH to 12-14, uses magnetic agitation 2h, mixed liquor is added polytetrafluoroethylene reactor and reacts 120 DEG C, 6h, and after naturally cooling to room temperature, centrifugal 20min washes 3 times, dries 12h for 50 DEG C subsequently, can obtain SnO 2/ MXene-Ti 3c 2composite material.

Claims (1)

1. the preparation method of graininess tin ash/two-dimensional nano titanium carbide composite material, is characterized in that, comprise the steps:
(1) by ternary layered Ti 3alC 2ceramic powder high-energy ball milling 1h-4h, rotating speed 400r/min, ratio of grinding media to material 10:1,40 DEG C-60 DEG C oven dry after refinement powder, obtain particle diameter at the Ti of 8 μm-75 μm 3alC 2ceramic powder;
(2) by gained Ti in step (1) 3alC 2ceramic powder gets 2g ~ 10g under 60 DEG C of conditions, is immersed in 50mL ~ 200mL35wt% ~ 45wt% hydrofluoric acid solution and reacts 6h ~ 120h; Stir, corrosion product is used deionized water eccentric cleaning, until centrifuged supernatant pH is between 5 ~ 6; Then washes of absolute alcohol is used 2 ~ 4 times; Gained solid sample is dry, obtain two-dimensional layer nano material MXene-Ti 3c 2;
(3) by SnCl 45H 2o, glucose and step (2) gained two-dimensional nano MXene-Ti 3c 2mixing, Sn 4+be 3:1, SnCl with the mol ratio of glucose 45H 2o and two-dimensional nano MXene-Ti 3c 2mass ratio is 2:1, using ethanol as solvent, uses NH 3h 2o regulates PH to 12-14, uses magnetic agitation 2h, mixed liquor is added polytetrafluoroethylene reactor and reacts 120 DEG C, 6h, and after naturally cooling to room temperature, centrifugal 20min washes 3 times, dries 12h for 50 DEG C subsequently, can obtain SnO 2/ MXene-Ti 3c 2composite material.
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CN105869910A (en) * 2016-05-31 2016-08-17 陕西科技大学 Composite material MoO3/Polyaniline/Ti3C2Tx and preparation method thereof
CN105870421A (en) * 2016-05-31 2016-08-17 陕西科技大学 C-SnO2/Ti3C2 two-dimensional-nanometer negative electrode material of lithium ion battery and preparation method thereof
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CN106057483A (en) * 2016-05-31 2016-10-26 陕西科技大学 Composite material MoO3/Ti3C2Tx and preparation method thereof
CN106082313A (en) * 2016-05-31 2016-11-09 陕西科技大学 The preparation method of bar-shaped tin ash/two-dimensional nano titanium carbide composite
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