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Temperature measurement method for crystallization heat treatment

A temperature measurement and crystallization technology, which is applied in measurement devices, material thermal analysis, instruments, etc., can solve the problems of unintuitive and inaccurate temperature, unknown maximum nucleation rate and temperature, etc., and achieve the effect of easy measurement and analysis.

Active Publication Date: 2017-11-14
CDGM OPTICAL GLASS
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] When existing glass or ceramics are subjected to crystallization heat treatment, the nucleation temperature and crystallization temperature are the temperature of glass transition temperature (Tg), sag temperature (Ts) and crystallization exothermic peak value by using differential thermal method or dilatometer. Measured to obtain, the differential thermal curve of the glass when it undergoes crystallization heat treatment is as follows figure 1 As shown, the nucleation temperature is generally set around Ts, or determined according to the nucleation temperature=Tg+2 / 3(Ts-Tg); the crystallization temperature is generally set near the crystallization peak, or according to the crystallization temperature=nucleation Temperature +100~150℃ is determined, so the temperature obtained is not intuitive and accurate. In addition, the maximum nucleation rate and its temperature are unknown, and the maximum nucleation rate temperature is always required for crystallization heat treatment of glass or ceramics. The important parameters obtained

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  • Temperature measurement method for crystallization heat treatment
  • Temperature measurement method for crystallization heat treatment
  • Temperature measurement method for crystallization heat treatment

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Experimental program
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Embodiment 1

[0028] Put the glass sample into the sample crucible of the thermal analysis instrument to test the glass sample. The glass sample is required to be melted evenly without devitrification, and the differential thermal curve of the glass at 5°C / min is obtained, and then the first-order differential analysis of the curve is carried out to obtain the differential thermal equation order differential curve, such as figure 2 shown.

[0029] 1) Determination of nucleation temperature and maximum rate of nucleation

[0030] From the differential thermal curve and first-order differential curve of the glass at 5°C / min, it can be seen that when the glass is heated to the sag temperature Ts, the energy reaches the activation energy required for the glass crystal nucleus, that is, the crystal nucleus begins to form, that is to say Phase separation begins; when the glass is heated to Ts1 * At this time, the first-order differential curve shows that heat absorption turns to heat release, ...

Embodiment 2

[0036] Put the glass sample into the sample crucible of the thermal analysis instrument, conduct the glass sample test, and obtain the differential thermal curve and the differential thermal first-order differential curve of the glass at 5°C / min, such as image 3 shown, from image 3 It can be seen that this glass material has three crystal forms.

[0037] From image 3 It can be seen that the first exothermic peak temperature Ts2 of the differential heat first-order differential curve * It can be used as the temperature to maximize the nucleation rate, which can be in Ts~Ts2 according to the crystal nucleus size * The selection of nucleation temperature in the temperature range; the onset temperature Ts3 of the second exothermic peak * is the lowest crystallization temperature of the first crystal form, and the peak temperature Ts4 *It can be used as the temperature to maximize the crystallization rate of the first crystal form, which can be set at Ts3 according to the cr...

Embodiment 3

[0040] Using the obtained nucleation temperature, nucleation rate maximization temperature and crystallization temperature of the method of the present invention, 3 kinds of glass samples (1# glass, 2# glass, 3# glass) are carried out to crystallization heat treatment process, to crystallization The processed sample is subjected to differential thermal analysis to obtain a 10°C / min differential thermal curve after glass crystallization, as shown in Figure 5 shown, from Figure 5 It can be seen that the glass is almost completely crystallized, and the desired crystal is obtained through the crystallization heat treatment process, such as Figure 6 , 7 , 8 shown.

[0041] From the analysis of the above theoretical and experimental measurement data, it can be concluded that the nucleation temperature, the maximum nucleation rate and the crystallization temperature obtained by the differential thermal first-order differential curve analysis method of the present invention are t...

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Abstract

The invention provides a method for measuring nucleation temperature and crystallization temperature intuitively during crystallization heat treatment. A temperature measurement method for crystallization heat treatment, the method comprising the following steps: 1) heating a material to obtain a differential thermal curve; 2) performing a first-order differential to the differential thermal curve to obtain a differential thermal first-order differential curve; 3) the differential thermal curve The first endothermic peak temperature Ts is the nucleation start temperature; the second exothermic peak start temperature Ts3* of the differential heat first differential curve is the lowest crystallization temperature. The present invention utilizes the differential thermal first-order differential analysis method to quickly and accurately obtain the nucleation temperature, maximum nucleation rate temperature, and crystallization temperature during crystallization heat treatment; the method of the present invention is intuitive, fast, easy to measure and analyze, and can also Use the data obtained from the analysis to carry out simulation process experiments to find the best nucleation and crystallization time, which has extremely important guiding significance for material crystallization.

Description

technical field [0001] The invention relates to a process for crystallization heat treatment of materials, in particular to a temperature measurement method for crystallization heat treatment of glass or ceramic materials. Background technique [0002] Glass-ceramics or ceramics are prepared by controlling the crystallization of glass or ceramics, which have breakthrough mechanical, thermal and electrical properties, while the external properties of the material depend on its internal structure. The transition temperature is closely related to the crystallization temperature. [0003] When existing glass or ceramics are subjected to crystallization heat treatment, the nucleation temperature and crystallization temperature are the temperature of glass transition temperature (Tg), sag temperature (Ts) and crystallization exothermic peak value by using differential thermal method or dilatometer. Measured to obtain, the differential thermal curve of the glass when it undergoes ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N25/14
Inventor 欧玲
Owner CDGM OPTICAL GLASS