Thermal analysis method of TiO2 crystallization by water supporting at low temperature

A low-temperature crystallization and thermal analysis technology, applied in the field of analysis and testing, can solve the problems of inability to obtain accurate phase transition temperature or phase transition time, difficult detection of crystalline phase transition peaks, and changing crystallization environment, so as to overcome the volatilization of water and prevent changes. , The effect of accurate thermal analysis method

Inactive Publication Date: 2014-05-28
NANJING NORMAL UNIVERSITY
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Problems solved by technology

At low temperature, TiO 2 The current main research method of water-assisted phase transition (Water assistant) is to use an oven to treat TiO2 at different temperatures. 2 The samples were treated isothermally, and then X-ray diffraction analysis was performed to determine the TiO 2 Whether phase change occurs, the process is very complicated, and the accurate phase change temperature or phase change time cannot be obtained
At present, no thermal analysis method has been used to study TiO 2 The literature reports of water-assisted crystallization at lower temperatures are mainly due to the fact that water is easy to volatilize during the heating process, which will change the TiO 2 crystallization environment; another reason is that moisture volatilization needs to absorb heat, TiO 2 When changing from amorphous crystal to anatase type, heat needs to be released, making it difficult to detect the tiny crystal phase transition peak

Method used

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  • Thermal analysis method of TiO2 crystallization by water supporting at low temperature
  • Thermal analysis method of TiO2 crystallization by water supporting at low temperature
  • Thermal analysis method of TiO2 crystallization by water supporting at low temperature

Examples

Experimental program
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Effect test

Embodiment 1

[0028] After careful selection, we choose Dow Corning silicone oil (DOW CORNING 200 FLUID, dynamic viscosity coefficient is 1000cst, density is 0.971kg / m 3 ) as an overlay.

[0029] Thermal analysis experiments were done on Diamond TG-DTA (Perkin-Elmer, USA). Weigh about 10mg of water, silicone oil, and water with silicone oil added as a covering layer, put them into a conventional aluminum oxide crucible without a cover, and raise the temperature to 85°C at a rate of 5°C / min, and use argon as a protective atmosphere during the heating process (purity 99.99%), the flow rate is 100ml / min.

[0030] The obtained TGA (Thermogravimetric Analysis, thermogravimetric analysis) data is processed as attached figure 1 As shown, it can be seen that if the pure water is not covered, it is basically completely volatilized when the temperature rises to 70°C, while the pure silicone oil is very stable before 85°C, with almost no weight loss. The pure water sample with silicone oil as the c...

Embodiment 2

[0033] Preparation of TiO by the classic sol-gel method 2 For nanomaterials, see Jean, J.H. and T.A. Ring, Nucleation and growth of monosized titania powders from alcohol solution. Langmuir, 1986. 2(2): p. 251-255. Hydroxypropyl cellulose (HPC 0.2g) was dissolved in anhydrous ethanol (50ml) and deionized water (0.3ml) solution, stirred for half an hour; added butyl titanate (TBOT, 97%, 0.85 ml), stirred Mix until it appears foggy, and age for 3 hours; finally centrifuge, wash 3 times with absolute ethanol, wash 1 time with water, and disperse in 20 ml of deionized water. The diameter of the synthesized original sample is about 200nm as detected by TEM, and its phase is amorphous as detected by XRD.

[0034] After careful selection, we choose Dow Corning silicone oil (DOW CORNING 200 FLUID, dynamic viscosity coefficient is 1000cst, density is 0.971kg / m 3 ) as an overlay.

[0035] Thermal analysis experiments were done on Diamond TG-DTA (Perkin-Elmer, USA). with conventional...

Embodiment 3

[0039] Preparation of TiO by the classic sol-gel method 2 aqueous solution. Hydroxypropyl cellulose (HPC 0.2g) was dissolved in anhydrous ethanol (50ml) and deionized water (0.3ml) solution, stirred for half an hour; added butyl titanate (TBOT, 97%, 0.85 ml), stirred Mix until it appears foggy, and age for 3 hours; finally centrifuge, wash 3 times with absolute ethanol, wash 1 time with water, and disperse in 20 ml of deionized water. The diameter of the synthesized original sample is about 200nm as detected by TEM, and its phase is amorphous as detected by XRD.

[0040] After careful selection, we choose Dow Corning silicone oil (DOW CORNING 200 FLUID, dynamic viscosity coefficient is 1000cst, density is 0.971kg / m 3 ) as an overlay.

[0041] Thermal analysis experiments were done on Diamond TG-DTA (Perkin-Elmer, USA). The same batch of water-wetted TiO prepared 2 After the samples were placed in 0H, 8H and 24H respectively, the conventional uncapped Al 2 o 3 Weigh abou...

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Abstract

The invention discloses a thermal analysis method of TiO2 crystallization by water supporting at low temperature, which is characterized in that a DTA or DSC method is used for determining a crystallization process of TiO2 under water infiltration condition. The method comprises the following steps: a cover layer is added on the surface of a solution sample to overcome the moisture volatilization during a determination process; detection sensitivity is increased by taking water and a covering substance as references, an isothermal crystallization mode is used, and the influence of TiO2 water infiltration temperature and infiltration time to the TiO2 crystallization phase transition by water supporting at low temperature can be researched according to an exothermic peak on an isothermal curve. According to the invention, the moisture volatilization of an aqueous solution sample during a heating process is effectively overcome, influence of the experimental environment to the experiment result is reduced, and the detection sensitivity of thermal analysis is increased. The operation of the thermal analysis method is convenient, the determination result is visual, and the thermal analysis method is the effective method for researching the TiO2 crystallization characteristic by water supporting at low temperature.

Description

technical field [0001] The invention belongs to the technical field of analysis and testing, and relates to a thermal analysis method, in particular to a TiO 2 Thermal analysis methods for water-assisted low-temperature crystallization. Background technique [0002] TiO 2 The representative porous metal oxide materials have received more and more attention due to their large specific surface area, and are widely used in supercapacitors, drug delivery, sensors, biomaterials and other fields. At the same time, the anatase TiO 2 As a typical photocatalytic oxidant, it is widely used in the treatment of environmental pollutants because of its advantages such as high activity, good stability, harmlessness to human body, and low source cost. [0003] TiO 2 The main crystal forms are anatase and rutile. Usually, with the increase of heat treatment temperature, TiO 2 The crystal phase structure changes from amorphous to anatase to rutile. Although many people have previously p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N25/14
Inventor 顾敏芬马青玉王昉李钢
Owner NANJING NORMAL UNIVERSITY
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