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Method for preparing self-support layered materials MXenes and application of self-support layered materials MXenes as Raman substrates

A layered material and self-supporting technology, which is applied in Raman scattering, material analysis, material excitation analysis, etc., can solve the problems of high price and complicated preparation process, and achieve the effect of low cost, simple preparation process and long application time limit

Active Publication Date: 2018-08-07
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these noble metal materials are not only expensive, but also complicated to prepare. Therefore, finding a cheap and stable SERS substrate material is the research focus in the field of Raman enhancement.

Method used

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  • Method for preparing self-support layered materials MXenes and application of self-support layered materials MXenes as Raman substrates
  • Method for preparing self-support layered materials MXenes and application of self-support layered materials MXenes as Raman substrates
  • Method for preparing self-support layered materials MXenes and application of self-support layered materials MXenes as Raman substrates

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1—Self-supporting layered material Ti 3 C 2 T x preparation of

[0037] Step 1. At 25°C, take 200 mesh Ti 3 AlC 2 1.0 g of the powder was dissolved in 10 ml of HF aqueous solution with a concentration of 40 wt% (40% by mass), and magnetically stirred for 2 h. Dilute the stirred suspension with deionized water, put it into a centrifuge at 1800rpm and centrifuge for 15min to obtain Ti 3 C 2 T x powder, and then wash the powder with deionized water until the pH of the centrifuged supernatant is 6-7. Use a filter to suction-filter the washed powder on the filter membrane, dry it in a blast drying oven at 50°C for 12 hours, and save it for other use.

[0038] Step 2, "insertion method" layered Ti 3 C 2 T x : Take part of the powder in step 1 and disperse it into a dimethyl sulfoxide (DMSO) solution at a ratio of 1g / 10ml (that is, 1g powder corresponds to 10ml DMSO) at 25°C, and stir magnetically for 18h. Centrifuge at 1800rpm for 15min to obtain Ti after ...

Embodiment 2

[0040] Embodiment 2, a kind of self-supporting layered material Ti 3 C 2 T x Compared with Example 1, the difference in the preparation method is that in step 1, magnetic stirring is performed for 4 hours, which corresponds to 2 hours of magnetic stirring in step 1.

[0041] figure 1 It is the two-dimensional Ti obtained by etching in Example 2 3 C 2 T x SEM photographs of the sheets. figure 2 It is the two-dimensional Ti obtained by etching in Example 2 3 C 2 T x The TEM photo of the layer, the number of layers is less than 10 layers. The prepared material is macroscopically composed of sheet material Ti 3 C 2 T x Composition, and two-dimensional Ti 3 C 2 T x The sheets are nano-layers, which are layered and dispersed through solvent intercalation to form Ti 3 C 2 T x nanolayers, forming a self-supporting structure.

[0042] image 3 for Ti 3 AlC 2 In the XRD patterns before and after etching, the (104) phase disappears after etching, and the intensity ...

Embodiment 3

[0043] Embodiment 3—Using the self-supporting layered material Ti prepared in embodiment 2 3 C 2 T x As a SERS substrate, rhodamine B is used as a Raman probe molecule, and the detection of rhodamine B molecular content includes the following steps:

[0044] Step 1. Use tweezers to take a small piece of the SERS substrate material and place it on a 1×1cm 2 On the silicon wafer, drop 6.5ul on the SERS substrate material with a concentration of 10 -5 The rhodamine B solution was volatilized in the air and dried to prepare a test sample for use.

[0045] Step 2. Place the detection sample prepared in step 1 in the Renishaw laser Raman spectrometer, wherein: the frequency range is 1710cm -1 —600cm -1 , the wavelength is 532nm, and the laser attenuation power is 0.01-0.05%. In the continuous mode, the Raman detection of Rhodamine B is completed with 2-5s exposure time and multiple acquisitions.

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Abstract

The invention discloses a method for preparing self-support layered materials MXenes and application of the self-support layered materials MXenes as Raman substrates. Ti3C2Tx which is prepared after Ti3AlC2 is etched by HF (hydrofluoric acid) is used as the SERS (surface enhanced Raman scattering) substrates, organic dye probe molecular solution with different degrees of concentration is coated onTi3C2Tx materials by the aid of dispensing processes, and then substrate materials with adsorbed probe molecules can be aired on glass slides to be used for Raman detection. The method and the application have the advantages that the Ti3C2Tx with a large specific surface area is excellent in adsorption performance for dye molecules, alkali metal ions and the like, and the quantities of hot spotscan be increased; the Ti3C2Tx substrates are good in homogeneity and high in stability and universality when used for detecting the dye molecules; the method for preparing the SERS substrates is simple and can have a broad application prospect in the field of food additives, pesticide residue detection and the like.

Description

technical field [0001] The invention belongs to the preparation of self-supporting layered nanomaterial MXene and its application in the field of surface-enhanced Raman, and relates to a high-concentration HF acid selective etching of Ti 3 AlC 2 The Al element in the phase obtains a self-supporting Ti 3 C 2 T x Preparation of membrane materials and their application as Raman substrates. Background technique [0002] Raman scattering spectroscopy is a detection and analysis technique that obtains molecular structure by studying molecular vibration and rotation information. However, the Raman scattering cross-section is small, and it is easily overwhelmed by some fluorescence during the detection process, which limits the application of Raman scattering. The discovery of surface-enhanced Raman scattering (SERS) overcomes the defect of small scattering cross-section, and can amplify Raman scattering signals by orders of magnitude. It has been widely used in physics, chemis...

Claims

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Application Information

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IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 薛涛周晓伟李方
Owner TIANJIN UNIV
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