CN111634913A - Stripping Ti3AlC2Preparation of high-purity few-layer Ti3C2Method of Tx slice - Google Patents
Stripping Ti3AlC2Preparation of high-purity few-layer Ti3C2Method of Tx slice Download PDFInfo
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Abstract
The invention discloses a stripping Ti3AlC2Preparation of high-purity few-layer Ti3C2TxAnd (3) a sheet layer method. By means of NaHF2Aqueous etching of Ti3AlC2Al layer in MAX phase powder while making Na+Inserted between layers to achieve one-step obtaining of Ti with a layer spacing of 12.35 Å (2 θ =7.1 °)3C2TxSheet layer, the process being HF, NH4HF2And HCl + LiF to obtain Ti3C2TxThe layer spacing is equalIs large. Ti obtained by stripping in the invention3C2TxThe lamella has an accordion-like structure, the lamella structure is complete and has larger particle size, and the generated by-product can pass through H2SO4Cleaning and removing, and the yield of the product can reach 80-85%; stripping off Ti3C2TxThe single-layer or few-layer Ti can be obtained by ultrasonic and centrifugal treatment of the lamella3C2Tx。
Description
Technical Field
The invention relates to a stripping Ti3AlC2Preparation of high-purity few-layer Ti3C2TxA lamellar method, belonging to the technical field of 2D nano material preparation.
Background
A novel two-dimensional nano material MXene is prepared by selecting proper etchant (such as HF, LiF + HCl, and NH) by using weak bonding force between A sheet layer and MX sheet layer in MAX phase4HF2) The A atomic layer in the MAX phase is degraded to prepare the novel carbon/nitride two-dimensional nano-layered material which has good conductivity and hydrophilicity. Which can be represented by the general formula Mn+1XnTxWherein T isxRepresenting functional groups (-OH, -F, -O, etc.) attached to MXene's surface resulting from chemical etching of the precursor MAX phase. And peeling off the multilayer MXene by means of ultrasonic oscillation or ball milling and the like, wherein the obtained monolayer or few-layer MXene is similar to Graphene (Graphene) in appearance. But compared with the monoatomic structure of graphene, the MX structure contains M and X diatoms or polyatomic atoms with better stability. In addition, the C and C atoms in the graphene are bonded singly, and M-X is a mixed valence bond of a covalent bond-an ionic bond-a metal bond, which also indicates that the M-X two-dimensional substance (MXene) has richer and more adjustable performance than the graphene. MXene has great application prospect in the fields of energy storage, electromagnetic interference shielding, transparent conductive coating, photo-thermal treatment, catalysis, water purification, antibacterial coating, lithium ion battery, super capacitor and the like due to excellent performance. Wherein, two-dimensional titanium carbide (Ti)3C2Tx) Is the most studied MXene. Thus, it is possible to provideIn the invention, Ti is selected3AlC2And etching is carried out.
To date, most MXene has been produced by etching the MAX phase with hydrofluoric acid (HF). Etched Ti3C2TxVarious polar organic molecules or large organic base molecules can be inserted, a single-layer or multi-layer MXene colloidal solution can be generated by mechanical vibration or ultrasonic treatment in water, and then the MXene lamella can be obtained by filtration. However, high concentrations of HF have a strong corrosive effect, can cause damage to the lamellae, and cannot achieve a one-step insertion of larger ions or molecules.
Feng et al [ reference: feng A, Yu Y, Jiang F, et al, contamination and commercial stability of NH4HF2-etched Ti3C2MXene[J]. Ceramics International,2017, 43(8):6322-6328.]It was found that NH was formed by epitaxial growth4HF2Can replace HF etching to prepare the film. But the method etches the obtained Ti3C2TxThe interlayer spacing is small and the product has impurities which are not easy to remove.
Zhang et al [ reference: zhang T, Pan L, Tang H, et al Synthesis Soft-dimensional Ti3C2TxMXene using HCl+LiF etchant: Enhanced exfoliation anddelamination[J]. Journal of Alloys&Compounds, 2016:S0925838816332455.]Production of Ti from lithium fluoride (LiF) and hydrochloric acid (HCl) solutions3C2TxThe method of (3) can reduce the use of HF, but the reaction produces aluminum-containing by-products which cannot be dissolved and removed during the washing process and remain in the sample. In addition, such processes generally require longer reaction times (up to 48 hours) to be obtained.
Disclosure of Invention
The present invention is to provide a stripped Ti3AlC2Preparation of high-purity few-layer Ti3C2TxMethod of using NaHF2Aqueous etching of Ti3AlC2The powder and the obtained product have potential application in the fields of super capacitors, lithium ion batteries, sodium ion batteries, sewage treatment, chemical adsorption and the like.
The invention realizes the stripping by a one-step method and the stripping at Ti3C2TxInterlayer insertion of Na+To enlarge the interlayer spacing without subsequent intercalation processing.
The invention provides a stripping Ti3AlC2Preparation of high-purity few-layer Ti3C2TxA method of sheeting comprising the steps of:
(1) weighing 1-2g of Ti3AlC2The powder is used as raw material and added with NaHF with the concentration of 1-5mol/L2Stirring and reacting in water solution at 30-100 deg.C for 5-15h, wherein the reaction is carried out under inert gas atmosphere, and Ti is mainly prevented3C2TxOxidation of the lamella;
(2) centrifugally cleaning the solution obtained in the reaction (1) by using deionized water, centrifuging at 3500 rpm for 2min, pouring out supernatant, continuously adding deionized water, and then dripping 8-10ml of concentrated H2SO4After 10-15min of reaction, the above centrifugation process (3500 rpm for 2 min) is repeated until the pH of the solution>5; finally, collecting the precipitate at the bottom of the centrifugal tube into a suction filtration funnel, adding deionized water into the suction filtration funnel, and collecting Ti by using a vacuum filtration method3C2TxDrying the powder in a vacuum drying oven for 10-20h at 60-80 deg.C;
(3) dispersing the product obtained in the reaction (2) in ethanol (CH) in sequence3CH2OH) and water (H)2O) solution, obtaining single-layer or few-layer Ti by centrifugation and ultrasound in reducing gas atmosphere3C2Tx. In the above process, the reaction formula of step (1) is
2Ti3AlC2+6NaHF2=2Ti3C2Tx+2Na3AlF6+3H2↑(1)
The reaction formula of the step (2) is
2Na3AlF6+6H2SO4=3Na2SO4+Al2(SO4)3+12HF↑ (2)
The HF gas obtained by the reaction in the reaction formula (2) can be collected and purified to prepare high-purity liquid HF.
Ti prepared by the above method3C2TxSheet layer, TxRepresents the surface functional groups-O, -F and-OH.
Ti prepared by the above method3C2TxThe sheet layer comprises the following elements in a mass ratio of Al to C to Ti to O to F = 1 to 4.69 to 2.67 to 3.58 to 5.54 to 2.32.
The method comprises the following steps: one-step method for realizing stripping and Ti3C2TxInterlayer insertion of Na+To enlarge the interlayer spacing without subsequent intercalation processing.
In the above process, NaHF2The concentration of the aqueous solution is 1-5mol/L, the reaction temperature is 30-100 ℃, and the reaction time is 5-15 h.
In the above method, Ti is added after etching off the Al layer3C2TxThe interlayer spacing of the lamella is 12.35 Å (2 theta =7.1 degrees), the lamella structure has an accordion-like structure, the integral grain diameter of the lamella structure is larger, and the byproduct generated by the reaction can pass through H2SO4And (3) cleaning and removing, as shown in equation (2).
Ti prepared by the above method3C2TxAnd the conductivity of the sheet layer is 2000-2500S/cm by using a four-point probe test.
Ti prepared by the above method3C2TxLamellar layer, the thermal stability is higher than that of Ti prepared by HF etching3C2TxLamellar, NaHF2Etched Ti3C2TxThe temperature at which the powder is completely converted to rutile is around 900 deg.c, while the transition temperature for HF etching is around 800 deg.c.
Ti prepared by the above method3C2TxThe adsorption capacity of the lamellar layer to the heavy metal Cu can reach 100-150 mg/g.
Ti prepared by the above method3C2TxThe lamella, ethanol and water are dispersed for five days without obvious falling.
The invention has the beneficial effects that:
compared with the prior art, the Ti prepared by the invention3C2TxThe lamella has an accordion-like structure, the particle size is large, the lamella structure is complete, solid by-products generated by the reaction can be cleaned and removed by sulfuric acid, and Ti3C2TxThe yield of the lamella can reach 80-85%, and the lamella has no obvious drop after being dispersed in ethanol and water for five days, and has higher conductivity, good thermal stability, heavy metal adsorption performance and the like. The invention provides a more convenient, faster and safer method for preparing MXene with excellent two-dimensional structure performance.
Drawings
FIG. 1 is the NaHF in example 12Aqueous solution successful etching of Ti3AlC2Then, Ti3C2TxSEM image of the lamella.
FIG. 2 is the NaHF in example 12Aqueous solution successful etching of Ti3AlC2Then, Ti3C2TxXRD pattern of the sheet.
FIG. 3 is the NaHF in example 12Aqueous solution successful etching of Ti3AlC2Then, XRD spectrum of the resultant was measured.
Detailed Description
The technical solution of the present invention is further described below with specific examples, but the scope of the present invention is not limited thereto.
The examples do not show the specific experimental steps or conditions, and the operation or conditions of the conventional experimental steps described in the literature in the field can be followed. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
50ml of deionized water were added to a 100ml polytetrafluoroethylene beaker, and 3g of NaHF was weighed2Pouring the powder into a beaker, heating and stirring in a water bath until the NaHF is added2The powder was completely dissolved. Weighing 1g of Ti3AlC2Powder addition of NaHF2In aqueous solution, then heated and stirred at 50 ℃ for 8h, and the reaction is carried out in N2The reaction is carried out in an atmosphere. Dissolving after reactionCentrifuging at 3500 rpm for 2min, removing supernatant, adding 50ml deionized water, and adding 8ml concentrated H2SO4After 10min of reaction, 3500 rpm was centrifuged for 5min, the supernatant was decanted and the centrifugation was repeated until the pH of the solution reached 5. Finally, adding the precipitate at the bottom of the centrifugal tube into deionized water and collecting Ti by using a vacuum filtration method3C2TxThe powder was then dried in a vacuum oven for 10h at 60 ℃.
Dried Ti3C2TxSEM image of the powder is shown in FIG. 1, where it can be seen that NaHF2The stripped lamella has an accordion-like structure, larger particle size and complete lamella structure, has no obvious lamella damage compared with the lamella obtained by HF etching with higher concentration, and the interlayer spacing can reach 12.35 Å (2 theta =7.1 degrees). As shown in figure 2, for Ti3AlC2And dried Ti3C2TxXRD analysis of the powder showed that 2 theta was shifted from 9.41 to 7.1 to the left, demonstrating increased interlayer spacing, Ti3AlC2The main characteristic peak at 39 ° disappeared, indicating that Al had been completely etched.
The material prepared in this example was characterized by X-ray powder diffraction from NaHF2Ti obtained by aqueous solution etching3C2TxThe interlayer spacing of the sheets was 12.35 Å (2 theta =7.1 deg.), which is larger than that obtained by one-step intercalation reported in the literature (Ti)3 AlC 22 θ =9.41 °, referred to the previous document: 2 θ =9.0 ° NH after HF etch4HF22 θ =8.5 °, 7.15 ° (two peaks present) after etching, 2 θ =8.6 ° after HCl + LiF etching.
Example 2
50ml of deionized water were added to a 100ml Teflon beaker, and 4g of NaHF were weighed2Pouring the powder into a beaker, heating and stirring in a water bath until the NaHF is added2The powder was completely dissolved. 1.5g of Ti were weighed3AlC2Powder addition of NaHF2In aqueous solution, then heated and stirred at 65 ℃ for 8h, and the reaction is carried out in N2The reaction is carried out in an atmosphere. The solution after the reaction was centrifuged and washed, and centrifuged at 3500 rpm2min, pouring out supernatant, adding 50ml deionized water, and dripping 9ml concentrated H2SO4After 12min of reaction, 3500 rpm was centrifuged for 5min, the supernatant was decanted and the centrifugation process was repeated until the pH of the solution reached 5. Finally, adding the precipitate at the bottom of the centrifugal tube into deionized water and collecting Ti by using a vacuum filtration method3C2TxThe powder was then dried in a vacuum oven for 15h at 70 ℃.
Example 3
50ml of deionized water were added to a 100ml Teflon beaker, and 5g of NaHF were weighed2Pouring the powder into a beaker, heating and stirring in a water bath until the NaHF is added2The powder was completely dissolved. Weighing 2g of Ti3AlC2Powder addition of NaHF2In aqueous solution, then heated and stirred at 80 ℃ for 8h, and the reaction is carried out in N2The reaction is carried out in an atmosphere. Centrifuging and cleaning the reacted solution at 3500 rpm for 2min, pouring out the supernatant, adding 50ml deionized water, and dripping 10ml concentrated H2SO4The reaction was carried out for 15min, centrifuged at 3500 rpm for 5min, the supernatant was decanted off, and the centrifugation process was repeated until the pH of the solution reached 5. Finally, adding the precipitate at the bottom of the centrifugal tube into deionized water and collecting Ti by using a vacuum filtration method3C2TxThe powder was then dried in a vacuum oven for 20h at 80 ℃.
Example 4
50ml of deionized water were added to a 100ml Teflon beaker, and 5g of NaHF were weighed2Pouring the powder into a beaker, heating and stirring in a water bath until the NaHF is added2The powder was completely dissolved. Weighing 2g of Ti3AlC2Powder addition of NaHF2In aqueous solution, then heated and stirred at 80 ℃ for 8h, and the reaction is carried out in N2The reaction is carried out in an atmosphere. The reacted solution was washed by centrifugation at 3500 rpm for 5min, and the centrifugation was repeated until the pH of the solution reached 5. Finally, adding the precipitate at the bottom of the centrifugal tube into deionized water and collecting Ti by using a vacuum filtration method3C2TxThe powder was then dried in a vacuum oven for 20h at 80 ℃. FIG. 3 is a drawing showingNaHF2Etching of Ti3AlC2Then has not passed through H2SO4The XRD spectrogram measured after cleaning obtains NaHF through Jade analysis2Etching of Ti3AlC2The latter being predominantly Ti3C2TxAnd Na3AlF6，Na3AlF6Can be mixed with H2SO4Reaction with H2SO4Will not be to Ti3C2TxThe damage to the lamella is effectively reduced3C2TxAl-containing compounds between the layers to further increase Ti3C2TxElectrochemical properties of the sheet.
Claims (9)
1. Stripping Ti3AlC2Preparation of high-purity few-layer Ti3C2TxA method of sheeting characterized by the steps of:
(1) weighing 1-2g of Ti3AlC2The powder is used as raw material, and NaHF with concentration of 1-5mol/L is added2Stirring and reacting in water solution at 30-100 deg.C for 5-15h, wherein the reaction is carried out in reducing gas atmosphere, and Ti is mainly prevented3C2TxOxidation of the lamella;
(2) centrifugally cleaning the solution obtained in the reaction (1) by using deionized water, centrifuging at 3500 rpm for 2min, pouring out supernatant, continuously adding deionized water, and then dripping 8-10ml of concentrated H2SO4After reacting for 10-15min, repeating the above centrifugation process until the pH of the solution is reached>5; finally, collecting the precipitate at the bottom of the centrifugal tube into a suction filtration funnel, adding deionized water into the suction filtration funnel, and collecting Ti by using a vacuum filtration method3C2TxDrying the powder in a vacuum drying oven for 10-20h at 60-80 deg.C;
(3) sequentially dispersing the product obtained in the reaction (2) in ethanol and aqueous solution, and obtaining single-layer or few-layer Ti by centrifugation and ultrasound in the atmosphere of reducing gas3C2Tx。
2. According to the claimsThe exfoliated Ti as described in claim 13AlC2Preparation of high-purity few-layer Ti3C2TxA process for producing a sheet characterized in that the reaction formula of step (1) is
2Ti3AlC2+6NaHF2=2Ti3C2Tx+2Na3AlF6+3H2↑(1)
The reaction formula of the step (2) is
2Na3AlF6+6H2SO4=3Na2SO4+Al2(SO4)3+12HF↑ (2)
The HF gas obtained by the reaction in the reaction formula (2) can be collected and purified to prepare high-purity liquid HF.
3. The exfoliated Ti of claim 13AlC2Preparation of high-purity few-layer Ti3C2TxA lamellar process, characterized in that, NaHF2The concentration of the aqueous solution is 1-5mol/L, the reaction temperature is 30-100 ℃, and the reaction time is 5-15 h.
4. The exfoliated Ti of claim 13AlC2Preparation of high-purity few-layer Ti3C2TxA process for the production of a sheet, characterized in that,
the reducing gases used in the step (1) and the step (3) are both N2。
5. A high purity Ti with few layers prepared by the method of any one of claims 1 to 53C2TxAnd (4) a sheet layer.
6. The high purity, few layer Ti of claim 53C2TxA sheet characterized by: t isxRepresents the surface functional groups-O, -F and-OH; obtained Ti3C2TxThe mass ratio of the elements in the sheet layer is Al to C to Ti to O to F to Na = 1 to 4.69 to 2.67 to 3.58 to 5.54 to 2.32.
7. The high purity, few layer Ti of claim 53C2TxA sheet characterized by: ti after etching off Al layer3C2TxThe interlayer spacing of the lamella is 12.35 Å, 2 theta =7.1 degrees, the lamella structure has an accordion-like structure, the integral grain diameter of the lamella structure is larger, and byproducts generated by the reaction pass through H2SO4Cleaning and removing, and the product yield can reach 80-85%.
8. The high purity, few layer Ti of claim 53C2TxA sheet characterized by: ti obtained by four-point Probe test3C2TxThe conductivity of the sheet layer was 2000-2500S/cm.
9. The high purity, few layer Ti of claim 53C2TxA sheet characterized by: the high-purity few-layer Ti3C2TxLamellar, heavy metal Cu2+The adsorption capacity of the catalyst can reach 100-150 mg/g.
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| CN113941366A (en) * | 2021-10-18 | 2022-01-18 | 太原理工大学 | Preparation method and antibacterial application of organic-inorganic hybrid two-dimensional photocatalytic composite material |
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| CN113941366A (en) * | 2021-10-18 | 2022-01-18 | 太原理工大学 | Preparation method and antibacterial application of organic-inorganic hybrid two-dimensional photocatalytic composite material |
| CN113941366B (en) * | 2021-10-18 | 2023-05-05 | 太原理工大学 | Preparation method and antibacterial application of organic-inorganic hybrid two-dimensional photocatalytic composite material |
| CN113896199A (en) * | 2021-11-23 | 2022-01-07 | 徐州纳烯新材料研究院有限公司 | Method for preparing MXene two-dimensional nanosheet through in-situ etching |
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