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Method for rapidly characterizing purity of titanium dioxide

A titanium dioxide and characterization technology, applied in the field of analysis and detection, can solve the problems of large contingency, inconsistent lithium intercalation, inaccurate calculation formula, etc., and achieve the effect of accurate phase content standard curve, improved accuracy, and wide application.

Active Publication Date: 2021-06-25
HUNAN UNIV
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Problems solved by technology

The shortcoming of this detection method is: (1) the establishment of standard curve is based on known sample ratio, can not use this method to establish content standard curve for the material that is difficult to obtain pure phase, should have limitation in application; ( 2) The single-point scanning Raman test is not statistical and has a large chance. The resulting content detection curve is not accurate enough, which affects the accuracy of the detection results
This detection method can use this method to establish a content standard curve for substances that are difficult to obtain pure phases. However, the disadvantages are: the lithium intercalation amount is inconsistent in different literature reports, and the electrochemical content calculation formula based on the lithium intercalation amount is inaccurate. Therefore, the sample content calculated by the electrochemical method cannot be used as the abscissa of the Raman standard curve, and there are big problems in the established Raman-based content detection curve, which affects the accuracy of the detection results.

Method used

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  • Method for rapidly characterizing purity of titanium dioxide
  • Method for rapidly characterizing purity of titanium dioxide
  • Method for rapidly characterizing purity of titanium dioxide

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Experimental program
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Effect test

Embodiment 1

[0045] Embodiment 1 Raman spectroscopy TiO 2 (A) Doped TiO 2 (B) content determination

[0046] One, the establishment of Raman spectral content standard curve mainly comprises the following steps:

[0047] 1. Synchrotron radiation XRD test

[0048] 6 unknown TiO 2 (A) content doped TiO 2 (B) The sample is subjected to synchrotron radiation XRD test, such as figure 1 , 2 As shown, samples 1 to 6TiO were obtained by Rietveld refinement 2 The serial content values ​​of (B) are respectively 60.727%, 78.523%, 98.759%, 99.999%, 98.245%, 95.511%, as shown in Table 1.

[0049] 2. Raman spectrum test

[0050] ① For TiO in step 1 2 (B) The sample adopts multi-site detection method, and adopts three surface scans, in which the area of ​​the surface scan is 9μm x 9μm, the number of points in each line of the surface scan is 30, and the number of lines of the surface scan is 30 lines. The Raman spectrum used Wavenumber range from 50 to 1000cm -1 , a total of 2700 spectra were o...

Embodiment 2

[0060] Embodiment 2 electrochemical method TiO 2 (A) Doped TiO 2 (B) content determination

[0061] One, the establishment of titanium dioxide purity standard curve mainly comprises the following steps:

[0062] 1. Synchrotron radiation XRD test

[0063] 6 unknown TiO 2 (A) content doped TiO 2 (B) The sample is subjected to synchrotron radiation XRD test, such as figure 1 , 2 As shown, samples 1 to 6TiO were obtained by Rietveld refinement 2 The serial content values ​​of (B) are respectively 60.727%, 78.523%, 98.759%, 99.999%, 98.245%, 95.511%, as shown in Table 1.

[0064] 2. Electrochemical characterization

[0065] ① Electrode sheet preparation: Mix the 6 samples in step 1 with conductive agent and binder at a ratio of 8:1:1, wherein the conductive agent is acetylene black, the binder is PVDF, and homogenize with a stirrer. Prepare the slurry. The slurry was coated on the copper foil current collector with a certain thickness, dried in vacuum at 100° C. for 12 ho...

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Abstract

The invention relates to a method for rapidly characterizing purity of titanium dioxide, and belongs to the technical field of analysis and detection. According to the method, on the basis of a TiO2 synchrotron radiation XRD detection result, a multiphase TiO2 content standard curve is established with data of a Raman spectroscopy method or an electrochemical characterization method respectively. According to a Raman spectrum detection method, the strongest characteristic peak of corresponding phase TiO2 is found in a Raman spectrogram, according to the electrochemical characterization, corresponding phase TiO2 lithium intercalation peaks are found in a capacity differential curve, peak areas are fitted respectively, the peak area of a to-be-detected phase is divided by the total peak area, the obtained ratio is used as a horizontal coordinate, the content refined by synchrotron radiation XRD is used as a vertical coordinate, and TiO2 content standard curves are respectively established so as to be a basis for quantitative detection of TiO2 with a unknown phase content. The method is suitable for quantitative determination of specified-phase TiO2 in multiphase TiO2; a standard curve is established based on data with statistical significance so that the detection result is more accurate; and two detection modes of Raman detection and electrochemical detection are provided, and an application field is wide.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, in particular to a titanium dioxide purity detection method based on synchrotron radiation XRD combined with Raman spectrum or electrochemical characterization. [0002] technical background [0003] Titanium dioxide, the chemical formula is TiO 2 , is an inorganic substance, and there are four phases at room temperature, namely the anatase phase TiO 2 (TiO 2 (A)), rutile phase TiO 2 (TiO 2 (R)), brookite phase TiO 2 , bronze phase TiO 2 (TiO 2 (B)), TiO 2 It has extensive and important applications in industry, medicine, food, cosmetics, environmental protection, etc., especially in the fields of energy and materials, TiO 2 It is a very promising anode material for lithium-ion batteries. Currently, TiO 2 The preparation methods of materials mainly include solvothermal method, ion exchange and solid state reaction method, etc., but pure phase TiO 2 The material is difficu...

Claims

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Application Information

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IPC IPC(8): G01N21/65G01N23/20G01N27/42
CPCG01N21/65G01N23/20G01N27/423
Inventor 刘继磊冉佳淼陈雨晴
Owner HUNAN UNIV
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