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Synthesis method of zirconium tungstate with minus thermal-expansion coefficient

A technology with a negative thermal expansion coefficient and a synthesis method, which is applied to tungsten compounds, zirconium compounds, chemical instruments and methods, etc., can solve problems such as chemical ratio mismatch, achieve low cost, and avoid exhaust gas pollution.

Inactive Publication Date: 2007-03-07
ZHENGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this method are: ① Since ZrW 2 o 8 The stable phase is in a very narrow temperature range of 1150-1257°C. Generally, the solid-state reaction sintering is carried out in the corresponding temperature range, and the preparation process generally takes 3-5 days to complete; ②ZrW 2 o 8 Decomposes into ZrO at 770-1050°C 2 and WO 3 , so it is usually cooled in liquid nitrogen immediately after being released from the furnace to reduce decomposition during cooling; ③WO 3 A large amount of volatilization in the long-term repeated sintering process will cause chemical ratio mismatch

Method used

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  • Synthesis method of zirconium tungstate with minus thermal-expansion coefficient
  • Synthesis method of zirconium tungstate with minus thermal-expansion coefficient
  • Synthesis method of zirconium tungstate with minus thermal-expansion coefficient

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Example 1, rapid sintering and synthesis of negative thermal expansion coefficient material ZrW 2 o 8 .

[0022] Weigh ZrO 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 1450° C., and the sintering time is 5 minutes. After sintering, put it into water to cool quickly. Composite material appears as a uniform green mass. XRD and Raman spectroscopy tests show that the synthetic material is α-phase zirconium tungstate, that is, α-phase ZrW 2 o 8 . The corresponding XRD and Raman spectra are shown in Figure 1(A) and Figure 1(B).

[0023] XRD analysis by and 、 , "Search-Match" and other XRD database comparisons are completed (the same below). X-ray Diffraction P...

Embodiment 2

[0026] Example 2, rapid sintering and synthesis of negative thermal expansion coefficient material ZrW 2 o 8 .

[0027] Weigh ZrO 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 1450 ° C, and the sintering time is 7 minutes. After sintering, put it into water to cool quickly. Composite material appears as a uniform green mass. XRD and Raman spectroscopy tests show that the synthetic material is α-phase zirconium tungstate, that is, α-phase ZrW 2 o 8 . The corresponding XRD and Raman spectra are shown in Figure 2(A) and Figure 2(B).

Embodiment 3

[0028] Example 3: rapid sintering and synthesis of negative thermal expansion coefficient material ZrW 2 o 8 .

[0029] Weigh ZrO 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 1400 ° C, and the sintering time is 10 minutes. After sintering, put it into water to cool quickly. Composite material appears as a uniform green mass. XRD and Raman spectroscopy tests show that the synthetic material is α-phase zirconium tungstate, that is, α-phase ZrW 2 o 8 . The corresponding XRD and Raman spectra are shown in Figure 3(A) and Figure 3(B).

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Abstract

The invention discloses a zirconium tungstate synthesizing method of negative heat-bulking coefficient material in the inorganic non-metal material synthetic technological domain, which comprises the following steps: blending ZrO2 and WO3 evenly with molar rate at 1:2-2.2; grinding the composite material for 60-120 min; sintering at 1280-1450 deg.c for 5-600min; cooling in the water rapidly.

Description

technical field [0001] The invention belongs to the technical field of material synthesis, in particular to a method for synthesizing zirconium tungstate, a negative thermal expansion coefficient material. 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 the dark side and t...

Claims

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Application Information

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IPC IPC(8): C01G41/00C01G25/00
Inventor 梁二军周鸿颖
Owner ZHENGZHOU UNIV
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