CN105470486B - The preparation method of graininess tin ash/two-dimensional nano carbonization titanium composite material - Google Patents

The preparation method of graininess tin ash/two-dimensional nano carbonization titanium composite material Download PDF

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CN105470486B
CN105470486B CN201510991800.9A CN201510991800A CN105470486B CN 105470486 B CN105470486 B CN 105470486B CN 201510991800 A CN201510991800 A CN 201510991800A CN 105470486 B CN105470486 B CN 105470486B
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CN105470486A (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 preparation method of graininess tin ash/two-dimensional nano carbonization titanium composite material, by ternary layered Ti3AlC2Ceramic powder ball milling；6h~120h is reacted in submergence in a solution of hydrofluoric acid；Stirring, gained solid sample is dried by corrosion product deionized water eccentric cleaning, obtains two-dimensional layer nano material MXene Ti3C2；By SnCl4·5H2O, glucose and two-dimensional nano MXene Ti3C2Mixing, using ethanol as solvent, PH to 12 14 is adjusted, with magnetic agitation 2h, react 120 DEG C, 6h, after naturally cooling to room temperature, centrifugation, drying can obtain SnO2/MXene‑Ti3C2Composite；Resulting materials of the present invention can effectively alleviate SnO2The bulk effect of nano particle, SnO2/MXene‑Ti3C2Nano composite material has fabulous application prospect in the negative material field of high storage germanium lithium ion battery.

Description

The preparation method of graininess tin ash/two-dimensional nano carbonization titanium composite material
Technical field
The invention belongs to nano-functional material preparation and its applied technical field, and in particular to graininess tin ash/bis- Tie up the preparation method of nano titanium carbide composite.
Background technology
Two-dimensional layer nano-carbide MXene-Ti3C2The material of a species graphene-structured, ultra-thin two-dimension nanometer sheet by In its unique appearance structure, less particle size, larger surface volume than the synusia thickness with atom level and with super Strong catalytic performance, photovoltaic performance and chemical property, in function ceramics, photocatalysis, lithium ion battery, solar cell, gas Body sensor etc. is widely used, but two-dimensional layer nano-carbide MXene-Ti3C2It is not easy directly to synthesize, And by Ti3AlC2Ceramic powder then turns into a kind of simple and easy method as predecessor to prepare.
Ternary layered Ti3AlC2Material possesses special crystal structure, is typical strong covalent bond between Ti and C, Al atoms It is weak metallic bond between layer inside and Al atoms and Ti, moreover, Al therein is easy to be corroded processing removing and obtain two-dimensional layer The Ti of shape class graphene-structured3C2,It is upper metal oxide-loaded herein, then it can realize the compound of material multiple functions and structure.
The oxide of tin is once considered as carbon negative pole material because being received much attention with height ratio capacity and low embedding lithium potential Most promising sub, but it is there is also some shortcomings, as volumetric expansion is up to more than 50% during first charge-discharge, follow Easily occur during the repeatedly embedded and abjection of lithium ion during ring " efflorescence " and " reunion " phenomenon, these result in the oxidation of tin Thing chemical property declines rapidly, so as to limit its extensive use in lithium ion battery.
Ma Weike et al. prepares graphene-based stannic oxide nanometer composite and have studied its chemical property, experiment knot Fruit shows that graphene-based tin ash significantly improves (Ma Weike .SnO as the charge/discharge capacity of lithium ion battery negative material2/ Graphene composite material Electrochemical Properties [D] the Yanshan Mountain:University On The Mountain Of Swallows, 2011.)；Zhu et al. is prepared using hydro-thermal method SnO2/ graphite nano composite materials and to show that it is better than in the performance of lithium ion battery, photocatalysis etc. single Grapheme material (Yun Guang Zhu, Ye Wang, Jian Xie, Gao-Shao Cao, Tie-Jun Zhu, Xinbing Zhao, Hui Ying Yang, Effects of Graphene Oxide Function Groups on SnO2/Graphene Nanocomposites for Lithium Storage Application, [J] .Electrochimica Acta.154 (2015) 338-344.) but the studies above are by SnO2It is supported on graphene, graphene can not effectively alleviate SnO2Body Product effect, and in Li+It is easily damaged during deintercalation.The present invention selects MXene-Ti3C2Two-dimensional layer material load SnO2, its It is typical strong covalent bond between middle Ti and C, can effectively alleviates SnO2Efflorescence reunite phenomena such as.Disadvantage mentioned above is improved, can Make tin ash/two-dimensional layer nano titanium carbide (MXene) composite, be expected in photocatalysis, wastewater treatment, lithium-ion electric There is good application in the fields such as pond, ultracapacitor, biology sensor.
The content of the invention
The defects of in order to overcome above-mentioned prior art, it is an object of the invention to provide the wiener of graininess tin ash/bis- The preparation method of rice carbonization titanium composite material, by hydro-thermal reaction by SnCl4·5H2O generates SnO under alkaline environment2Load to MXene-Ti3C2Nano-material surface, so as to provide a kind of graininess tin ash/two-dimensional nano titanium carbide (MXene) composite wood The preparation method of material；First by the Ti after synthesis and processing3AlC2Powder carries out chemical etching in HF acid, makes Al by selectivity Etch away, form a kind of two-dimensional layer material MXene-Ti3C2, then in two-dimensional layer material MXene-Ti3C2Upper load SnO2, Make MXene-Ti3C2Ratio surface it is bigger, taken into account SnO2The advantages of, such as photocatalysis performance, one's own physical property, pattern is various etc..
In order to achieve the above object, technical scheme is as follows：
The preparation method of graininess tin ash/two-dimensional nano carbonization titanium composite material, it is characterised in that including following step Suddenly：
(1) ternary layered Ti is prepared first according to patent ZL201310497696.9 method3AlC2Ceramic 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 of -60 DEG C of drying after powder are refined, obtain particle diameter In 8 μm -75 μm of Ti3AlC2Ceramic powder；
(2) by gained Ti in step (1)3AlC2Ceramic powder takes 2g~10g under the conditions of 60 DEG C, be immersed in 50mL~ 6h~120h is reacted in 200mL 35wt%~45wt% hydrofluoric acid solutions；Stirring, corrosion product is centrifuged clearly with deionized water Wash, until centrifuged supernatant pH is between 5~6；Then washes of absolute alcohol is used 2~4 times；Gained solid sample is dried, obtained To two-dimensional layer nano material MXene-Ti3C2；
(3) by SnCl4·5H2O, glucose and step (2) gained two-dimensional nano MXene-Ti3C2Mixing, Sn4+With Portugal The mol ratio of grape sugar is 3:1, SnCl4·5H2O and two-dimensional nano MXene-Ti3C2Mass ratio is 2：1, using ethanol as solvent, Use NH3·H2O adjusts PH to 12-14, with magnetic agitation 2h, mixed liquor is added into ptfe autoclave and reacts 120 DEG C, 6h, After naturally cooling to room temperature, centrifugation 20min is washed 3 times, subsequent 50 DEG C of drying 12h, you can obtain SnO2/MXene-Ti3C2It is compound Material.
Advantage of the invention is that utilize a step hydro-thermal reaction so that SnO2Uniform load is in MXene-Ti3C2On, prepare Obtain the various SnO of pattern2/MXene-Ti3C2Composite.And SnO2/MXene-Ti3C2Composite has excellent electricity Chemical property, during as lithium ion battery negative material, discharge capacity may be up to 1030mAh g first for it-1So that two-dimensional layer Nano material MXene-Ti3C2A new situation is opened in the application aspect of lithium ion battery, its good thermal conductivity and conduction Performance has played huge effect.
The present invention selects MXene-Ti3C2Two-dimensional layer material load SnO2, it is typical strongly covalent between wherein Ti and C Key, it can effectively alleviate SnO2Efflorescence reunite phenomena such as.Capacitance is effectively improved, is up to its first charge-discharge capacity 1030.1mAh g-1.Work compared to forefathers all improves significantly, and can make tin ash/two-dimensional layer nano titanium carbide (MXene) composite, it is expected to have more preferable application in fields such as lithium ion battery, ultracapacitors.
Brief description of the drawings
Fig. 1 is Ti3AlC2After powder corrosion treatment, and corrosion product MXene-Ti3C2Load SnO2The XRD spectrum of sample.
Fig. 2 (a) is Ti3AlC2The SEM figures of powder granule, Fig. 2 (b) are MXene-Ti after corrosion treatment3C2SEM figure, figure 2 (c) is SnO2/MXene-Ti3C2The SEM figures of nano composite material, Fig. 2 (d) is SnO2/MXene-Ti3C2Nano composite material Local high power SEM figure.
Embodiment
The present invention is further described below by way of specific embodiment, the present invention can not depart from the present invention by others yet The scheme of technical characteristic describes, therefore all changes within the scope of the present invention or in the equivalent scope of the invention are of the invention Comprising.
Embodiment one
The present embodiment comprises the following steps：
(1) the ternary layered Ti of high-purity is prepared using the method for vacuum-sintering3AlC2Ceramic powder, then high energy ball Be milled body 4h, rotating speed 400r/min, ratio of grinding media to material 10:1, refine 60 DEG C of drying after powder.SEM figures are shown from Fig. 2 (a) Ti3AlC2The microscopic appearance of crystal, it can be seen that its grain size is about 8 μm, and its obvious layer structure；
(2) gained powder 2g in step (1) under the conditions of 60 DEG C, is immersed in 100mL40% hydrofluoric acid solutions and reacted 48h, stirring, by corrosion product deionized water eccentric cleaning, until centrifuged supernatant pH=5；Then washes of absolute alcohol 3 is used It is secondary；By gained solid sample drying at room temperature, two-dimensional layer nano material MXene-Ti is obtained3C2, see Fig. 2 (b), wherein SEM figures show MXene-Ti is shown3C2Microscopic appearance, it can be seen that its lamellar spacing is about 50nm, is typical two-dimensional layer nano material；
(3) hydro-thermal reaction so that Sn4+Mol ratio with glucose is 3:1, by SnCl4·5H2O and step (2) gained two Wiener rice MXene-Ti3C2With 2：1 mass ratio mixing, using ethanol as solvent, uses NH3·H2O adjusts PH to 12-14, uses magnetic Power stirs 2h, and mixed liquor is added into ptfe autoclave reacts 120 DEG C, 6h, after naturally cooling to room temperature, centrifuges 20min Washing 3 times, subsequent 50 DEG C of drying 12h, you can obtain SnO2/MXene-Ti3C2Composite.It is visible from Fig. 1 XRD spectrums SnO2-Ti3C2Contain SnO in powder2And Ti3C2Composition.See Fig. 2 (c) and (d), wherein SEM figures show SnO2/MXene- Ti3C2The microscopic appearance of composite, it can be seen that SnO2Size is about 25nm, and is evenly distributed, and loads to MXene- well Ti3C2In two-dimensional layer nano material, the SnO of novelty is formed2/MXene-Ti3C2Nano composite material.
Embodiment two：
The present embodiment comprises the following steps:
(1) the ternary layered Ti of high-purity is prepared using the method for vacuum-sintering3AlC2Ceramic powder, then high energy ball Be milled body 1h, rotating speed 400r/min, ratio of grinding media to material 10:1,40 DEG C of drying after powder are refined, obtain Ti3AlC2Ceramic powder；
(2) gained powder 2g in step (1) under conditions of 60 DEG C, is immersed in 50mL35% hydrofluoric acid solutions and reacted 6h, stirring, it is about 5~6 that deionized water, which is cleaned to pH, washes of absolute alcohol 2 times, centrifuges, gained solid sample is dried, Obtain two-dimensional layer MXene-Ti3C2Nano material；
(3) by SnCl4·5H2O, glucose and step (2) gained two-dimensional nano MXene-Ti3C2Mixing, Sn4+With Portugal The mol ratio of grape sugar is 3:1, SnCl4·5H2O and two-dimensional nano MXene-Ti3C2Mass ratio is with 2：1, using ethanol as solvent, Use NH3·H2O adjusts PH to 12-14, with magnetic agitation 2h, mixed liquor is added into ptfe autoclave and reacts 120 DEG C, 6h, After naturally cooling to room temperature, centrifugation 20min is washed 3 times, subsequent 50 DEG C of drying 12h, you can obtain SnO2/MXene-Ti3C2It is compound Material.
Embodiment three
The present embodiment comprises the following steps：
(1) the ternary layered Ti of high-purity is prepared using the method for vacuum-sintering3AlC2Ceramic powder, then high energy ball Be milled body 3h, rotating speed 400r/min, ratio of grinding media to material 10:1, refine 50 DEG C of drying after powder；
(2) gained powder 3g in step (1) under conditions of 60 DEG C, is immersed in 70mL35% hydrofluoric acid solutions and reacted 24h, stirring, by corrosion product deionized water eccentric cleaning, until centrifuged supernatant pH is between 5~6；Then with anhydrous second Alcohol cleans 3 times；Gained solid sample is dried, obtains two-dimensional layer nano material MXene-Ti3C2；
(3) by SnCl4·5H2O, glucose and step (2) gained two-dimensional nano MXene-Ti3C2Mixing, Sn4+With Portugal The mol ratio of grape sugar is 3:1, SnCl4·5H2O and two-dimensional nano MXene-Ti3C2Mass ratio is with 2：1, using ethanol as solvent, Use NH3·H2O adjusts PH to 12-14, with magnetic agitation 2h, mixed liquor is added into ptfe autoclave and reacts 120 DEG C, 6h, After naturally cooling to room temperature, centrifugation 20min is washed 3 times,
Subsequent 50 DEG C of drying 12h, that is, can obtain SnO2/MXene-Ti3C2Composite.
Example IV
The present embodiment comprises the following steps：
(1) the ternary layered Ti of high-purity is prepared using the method for vacuum-sintering3AlC2Ceramic powder, then high energy ball Be milled body 3h, rotating speed 400r/min, ratio of grinding media to material 10:1, refine 50 DEG C of drying after powder；
(2) gained powder 4g in step (1) under conditions of 60 DEG C, is immersed in 90mL40% hydrofluoric acid solutions and reacted 48h, stirring, by corrosion product deionized water eccentric cleaning, until centrifuged supernatant pH is between 5~6；Then with anhydrous second Alcohol cleans 4 times；Gained solid sample is dried, obtains two-dimensional layer nano material MXene-Ti3C2；
(3) by SnCl4·5H2O, glucose and step (2) gained two-dimensional nano MXene-Ti3C2Mixing, Sn4+With Portugal The mol ratio of grape sugar is 3:1, SnCl4·5H2O and two-dimensional nano MXene-Ti3C2Mass ratio is with 2：1, using ethanol as solvent, Use NH3·H2O adjusts PH to 12-14, with magnetic agitation 2h, mixed liquor is added into ptfe autoclave and reacts 120 DEG C, 6h, After naturally cooling to room temperature, centrifugation 20min is washed 3 times, subsequent 50 DEG C of drying 12h, you can obtain SnO2/MXene-Ti3C2It is compound Material.

Claims (1)

1. the preparation method of graininess tin ash/two-dimensional nano carbonization titanium composite material, it is characterised in that including following step Suddenly：
(1) by ternary layered Ti3AlC2Ceramic powder high-energy ball milling 1h-4h, rotating speed 400r/min, ratio of grinding media to material 10:1, refine powder 40 DEG C of -60 DEG C of drying afterwards, obtain Ti of the particle diameter at 8 μm -75 μm3AlC2Ceramic powder；
(2) by gained Ti in step (1)3AlC2Ceramic powder takes 2g~10g to be immersed in 50mL~200mL under the conditions of 60 DEG C 6h~120h is reacted in 35wt%~45wt% hydrofluoric acid solutions；Stirring, by corrosion product 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 dried, obtains two-dimensional layer Shape nano material MXene-Ti3C2；
(3) by SnCl4·5H2O, glucose and step (2) gained two-dimensional layer nano material MXene-Ti3C2Mixing, Sn4+ Mol ratio with glucose is 3:1, SnCl4·5H2O and two-dimensional layer nano material MXene-Ti3C2Mass ratio is 2：1, with second Alcohol uses NH as solvent3·H2O adjusts PH to 12-14, and with magnetic agitation 2h, it is anti-that mixed liquor is added into ptfe autoclave 120 DEG C, 6h, after naturally cooling to room temperature are answered, centrifugation 20min is washed 3 times, subsequent 50 DEG C of drying 12h, you can obtain graininess two Tin oxide/two-dimensional nano carbonization titanium composite material.
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