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Negative heat expansion coefficient material quick sintering synthesizing method

A technology with a negative thermal expansion coefficient and a synthesis method, which is applied in the field of material synthesis, can solve the problems of long high-temperature sintering time, complicated preparation process, and long time consumption, and achieve the effects of fast synthesis speed, avoiding exhaust gas pollution, and low energy consumption

Inactive Publication Date: 2009-10-28
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] From the above, it can be seen that the traditional solid state reaction method takes a long time to sinter at high temperature and consumes a lot of energy. The sample preparation time generally takes a few days to about a week, and the total time is long.
Long time sintering causes WO 3 and MO 3 The large amount of volatilization is another shortcoming of the traditional solid state reaction method
However, the liquid phase synthesis method mostly uses salt compounds as raw materials and reacts in solvents (often need to add acid reagents). The preparation process is complicated and time-consuming, and the prepared precursor still needs to be sintered at high temperature.

Method used

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  • Negative heat expansion coefficient material quick sintering synthesizing method
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  • Negative heat expansion coefficient material quick sintering synthesizing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1, rapid sintering synthesis negative thermal expansion coefficient material Hf (WO 4 ) 2 :

[0044] Weigh HfO at a molar ratio of 1:2.15 2 with WO 3 , mixed and ground for 90 minutes, the mixture was compacted, and then sintered and synthesized in a high-temperature furnace. The synthesis process parameters are: ECFK-10-14 high-temperature sintering furnace produced by Shanghai Guangyi High-temperature Technology Industry Co., Ltd., the sintering temperature is 1300 ° C, and the sintering time is 300 minutes. After sintering, put it into water to cool quickly. XRD and Raman spectroscopy tests show that the synthesized material is cubic phase hafnium tungstate, namely α-Hf(WO 4 ) 2 . The corresponding XRD and Raman spectra are shown in Figure 1(A) and Figure 1(B).

[0045] XRD analysis by and 、 , "Search-Match" and other XRD database comparisons are completed (the same below). X-ray diffraction phase analysis showed that the synthesized material Hf...

Embodiment 2

[0048] Embodiment 2, rapid sintering synthesis negative thermal expansion coefficient material Hf (WO 4 ) 2 :

[0049] Weigh HfO at a molar ratio of 1:2.2 2 with WO 3 , mixed and ground for 90 minutes, the mixture was compacted, and then sintered and synthesized in a high-temperature furnace. The synthesis process parameters are: ECFK-10-14 high-temperature sintering furnace produced by Shanghai Guangyi High-temperature Technology Industry Co., Ltd., the sintering temperature is 1300 ° C, and the sintering time is 180 minutes. After sintering, put it into water to cool quickly. XRD and Raman spectroscopy tests show that the synthetic material is α-phase hafnium tungstate, namely α-Hf(WO 4 ) 2 . The corresponding XRD and Raman spectra are shown in Figure 2(A) and Figure 2(B).

Embodiment 3

[0050] Embodiment 3: rapid sintering synthesis negative thermal expansion coefficient material Hf (WO 4 ) 2 :

[0051] Weigh HfO at a molar ratio of 1:2.2 2 with WO 3 , mixed and ground for 90 minutes, the mixture was compacted, and then sintered and synthesized in a high-temperature furnace. The synthesis process parameters are: ECFK-10-14 high-temperature sintering furnace produced by Shanghai Guangyi High-temperature Technology Industry Co., Ltd., the sintering temperature is 1300 ° C, and the sintering time is 60 minutes. After sintering, put it into water to cool quickly. XRD and Raman spectroscopy tests show that the synthetic material is α-phase hafnium tungstate, namely α-Hf(WO 4 ) 2 . The corresponding XRD and Raman spectra are shown in Figure 3(A) and Figure 3(B).

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Abstract

The rapid sintering synthesis method of materials with negative thermal expansion coefficients is to sinter the raw materials that can generate negative thermal expansion coefficient materials in a high-temperature furnace, so that they can quickly react to form negative thermal expansion coefficient materials. The material with negative thermal expansion coefficient is Hf(WO4)2, the raw materials used are HfO2 and WO3, the molar ratio of HfO2 to WO3 is 1:2-2.2; the sintering temperature is 1300°C-1460°C, and the sintering time is 5 minutes to 300 minutes . The negative thermal expansion coefficient material is Hf(MoO4)2, the raw materials used are HfO2 and MoO3, the molar ratio of HfO2 and MoO3 is 1:2-2.2; the sintering temperature is 800°C-1150°C, and the sintering time is 5 minutes to 300 minutes . The material with negative thermal expansion coefficient is Zr(MoO4)2, the raw materials used are ZrO2 and MoO3, the molar ratio of ZrO2 and MoO3 is 1:2-2.2; the sintering temperature is 900°C-1200°C, and the sintering time is 5 minutes to 120 minutes . The invention has high synthesis speed, low energy consumption, no pollution, high purity and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of material synthesis, and in particular relates to a rapid sintering synthesis method of negative thermal expansion coefficient materials. Background technique [0002] The rapid sintering synthetic material technology uses a high-temperature sintering furnace as a heating source, and the raw material components react at high temperature in the sintering furnace to form new materials. Most materials have the property of thermal expansion and contraction, and the thermal stress (or thermal shock wave) generated by thermal expansion and contraction is often the main reason for device fatigue, performance degradation, failure or even fracture and shedding. In the field of aerospace, both functional and structural materials are faced with the severe test of thermal stress (or thermal shock wave). When a spacecraft is in space, it is irradiated by the sun, and the temperature difference between its dark and sunn...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/64C04B35/50C04B35/495
Inventor 梁二军袁斌周鸿颖
Owner ZHENGZHOU UNIV
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