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Sintering and synthesizing method of negative thermal expansion material Zr2P2MO12

A negative thermal expansion material, zr2p2mo12 technology, applied in the field of inorganic non-metallic materials, can solve the problems of sample contamination in the sintering process, time-consuming material preparation, complicated preparation process, etc., achieve high purity, avoid ammonia emission problems, and simple reaction process Effect

Inactive Publication Date: 2010-11-24
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In existing reports, the commonly used preparation method for this type of material is the solid phase reaction method [Gregory A.Merkel et al.United States, US6377729B2; Mehmet Cetinkol et al.Journal of Solid State Chemistry 182(2009) 1304-1311], Although this method can produce high-purity Zr 2 P 2 MO 12 Similar to negative expansion materials, but there are disadvantages such as complicated preparation process, long time consumption and high energy consumption
Especially in the preparation of Zr 2 P 2 MO 12 NH is selected as the raw material 4 h 2 PO 4 Provide P 5+ Ions, need to be pretreated at a certain temperature before sintering in order to release the NH 3 , usually requires multiple sintering (sintering-grinding-re-sintering), which may contaminate the sample and complicate the sintering process, material preparation takes a long time and consumes a lot of energy

Method used

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  • Sintering and synthesizing method of negative thermal expansion material Zr2P2MO12
  • Sintering and synthesizing method of negative thermal expansion material Zr2P2MO12
  • Sintering and synthesizing method of negative thermal expansion material Zr2P2MO12

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Experimental program
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Effect test

Embodiment 1

[0030] Set the high-temperature tube furnace to heat up to the sintering temperature of 1200°C at a rate of 5°C / min:

[0031] will be able to generate Zr 2 P 2 WO 12 Raw material ZrO 2 、WO 3 ,P 2 o 5Weigh it at a molar ratio of 2:1:1, grind it in an agate mortar for 2 hours, and mix the raw materials evenly; put the ground and mixed raw materials in a drying oven for 4 hours, and the temperature of the drying oven is 150°C; The hydraulic machine presses the dried raw material powder into a disc shape with a size of 2cm in diameter and 2mm in thickness. After pressing, put it into a sealed bag quickly to prevent the sample from absorbing water and pulverize it for later use; finally put it in a high temperature that has been heated to 1200°C Sinter in a tube furnace for 80min, take it out after sintering, and let it cool naturally at room temperature.

[0032] For the X-ray diffraction phase analysis corresponding to the product, see figure 1 , figure 1 The XRD results...

Embodiment 2

[0034] The difference from Example 1 is: a high-temperature tube furnace is set to heat up to a sintering temperature of 1300° C., and the sintering time is 1 h; ZrO 2 : WO 3 :P 2 o 5 The molar ratio of Zr is 2:1.1:1.1; the drying temperature is 160°C, and the drying time is 3h+40min; the formed Zr 2 P 2 WO 12 For the corresponding X-ray diffraction phase analysis see figure 2 , figure 2 The XRD results showed the formation of pure Zr 2 P 2 WO 12 Mutually.

Embodiment 3

[0036] The difference from Example 1 is that a high-temperature tube furnace is set to heat up to a sintering temperature of 1300°C, and the sintering time is 2h; ZrO 2 : WO 3 :P 2 o 5 The molar ratio is 2:1.1:1.1; the drying temperature is 170°C, and the drying time is 3h+20min; the formed Zr 2 P 2 WO 12 For the corresponding X-ray diffraction phase analysis see image 3 , image 3 The XRD results showed the formation of pure Zr 2 P 2 WO 12 Mutually.

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Abstract

The invention discloses a sintering and synthesizing method of negative thermal expansion material Zr2P2MO12, belonging to the field of inorganic nonmetallic materials. The negative thermal expansion material has a molecular formula as follows: Zr2P2MO12, wherein M is W or Mo. The method is characterized by comprising the following steps: taking materials based on that a mole ratio of ZrO2 to WO3 to P2O5 or ZrO2 to MoO3 toP2O5 of 2:(1-1.2): (1-1.2), grinding and evenly mixing, and directly sintering the mixed raw materials or sintering the mixed raw materials after tabletting. The invention uses the high temperature rapid sintering and synthesizing method to prepare the negative thermal expansion material Zr2P2MO12 and takes P2O5 as the raw material, thereby avoiding discharge of redundant ammonia and reducing pollution; and the negative thermal expansion material can be sintered for one time at the same time. The invention has the advantages that the reaction process is simple, the sintering speed is rapid, and the sintering time is short; and the raw materials can fully react at high temperature, and the produced product has high purity.

Description

technical field [0001] The invention belongs to the field of inorganic non-metallic materials, in particular to a negative thermal expansion material Zr 2 P 2 MO 12 sintering synthesis method. Background technique [0002] Negative expansion materials, in a certain temperature range, have a negative average thermal expansion coefficient and have the characteristics of "heat shrink and cold expand", and have potential important uses in many fields such as optics, electronics, medicine, machinery, and aviation. As far as the current situation is concerned, although negative expansion materials have gradually attracted everyone's attention, the research on this type of material is not perfect, and it has not been applied on a large scale so far. There are still many problems to be solved, such as the selection of raw materials, relative Changes, improvements in mechanical properties, complex production processes, etc. Currently, commonly studied negative expansion materials...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/48C04B35/495C04B35/622
Inventor 梁二军胡庆伦商瑞
Owner ZHENGZHOU UNIV
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