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Negative thermal expansion material and composite material containing the negative thermal expansion material

A technology of negative thermal expansion material and expansion material, applied in the direction of phosphorus compounds, fibrous fillers, chemical instruments and methods, etc., can solve the problem of no spherical zirconium tungstate phosphate reported, and achieve excellent filling characteristics and excellent dispersibility. Effect

Active Publication Date: 2021-03-09
NIPPON CHECMICAL IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, according to patent documents 1 and 2 and non-patent document 1, the particle shape of zirconium phosphate tungstate produced is broken, and as far as the inventors of the present invention know, there is no report of spherical zirconium phosphate tungstate

Method used

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  • Negative thermal expansion material and composite material containing the negative thermal expansion material
  • Negative thermal expansion material and composite material containing the negative thermal expansion material
  • Negative thermal expansion material and composite material containing the negative thermal expansion material

Examples

Experimental program
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Embodiment

[0114] Hereinafter, the present invention will be described in more detail using examples, but the scope of the present invention is not limited to these examples.

[0115]

[0116] 1. X-ray diffraction analysis: The X-ray diffraction analysis of zirconium phosphate tungstate and the reaction precursor used Rigaku's Ultima IV. Use Cu-Kα as the radiation source. The measurement conditions are: tube voltage 40kV, tube current 40mA, scanning speed 0.1° / sec.

[0117] 2. Infrared absorption spectrum (FT-IR) analysis: The infrared absorption spectrum analysis of the reaction precursor uses NICOLET 6700 produced by ThermoFisher Scientific, with a resolution of 4cm －1 , Cumulative number: 256 times, measuring wave number range: 400cm －1 ~4000cm －1 conditions are measured. The ATR method is used for measurement, and ATR correction and spectrum smoothing are performed.

[0118] 3. Average particle diameter: The average particle diameter of each raw material and solid content in t...

reference example 1

[0121] Commercially available tungsten trioxide (WO 3 , average particle diameter 1.2 μm) 15 parts by mass were added to the beaker, 84 parts by mass of pure water was added, and 1 part by mass of ammonium polycarboxylic acid salt was added as a dispersant.

[0122] It stirred at room temperature (25 degreeC) for 120 minutes using the Three-One Motor mixer, and prepared the 15 mass % slurry containing tungsten trioxide. The average particle diameter of the solid content in the slurry was 1.2 μm.

[0123] Then, add zirconium hydroxide and 85% by mass phosphoric acid aqueous solution to the slurry at room temperature (25° C.), so that the molar ratio of Zr in the slurry: W: P reaches 2.00: 1.00: 2.00, and carry out 2 steps under stirring. hour response.

[0124] After completion of the reaction, all the slurry was dried at 200° C. under the atmosphere for 24 hours to obtain a reaction precursor. The obtained reaction precursor is carried out X-ray diffraction, the result only...

Embodiment 1

[0128] Commercially available tungsten trioxide (WO 3 , average particle size 1.2 μm) 15 parts by mass were added to the beaker, and 84 parts by mass of pure water was added.

[0129] It stirred at room temperature (25 degreeC) for 120 minutes, and prepared the 15 mass % slurry containing tungsten trioxide. The average particle diameter of the solid content in the slurry was 1.2 μm.

[0130] Next, zirconium hydroxide, 85% by mass phosphoric acid aqueous solution, and magnesium hydroxide were added to the slurry at room temperature (25°C) so that the molar ratio of Zr:W:P:Mg in the slurry became 2.00:1.00:2.00 : 0.1, after that, the temperature was raised to 80° C., and the reaction was carried out for 4 hours under stirring.

[0131] After completion of the reaction, add 1 part by mass of polyhydric carboxylic acid ammonium salt as a dispersant, and while stirring the slurry, supply it to a media-stirred bead mill with zirconia beads with a diameter of 0.5 mm, and mix for 15...

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Abstract

An object of the present invention is to provide a negative thermal expansion material having excellent dispersibility and filling properties relative to positive thermal expansion materials. The method that the present invention solves the problem is: the negative thermal expansion material of the present invention contains BET specific surface area and is 2m 2 / g spherical zirconium tungstate phosphate. The sphericity is preferably not less than 0.90 and not more than 1. It is also preferable to further contain at least Mg and / or V as subcomponent elements. It is also preferable that the content of subcomponent elements is 0.1 mass % or more and 3 mass % or less. It is also preferable that the average particle diameter is not less than 1 μm and not more than 50 μm.

Description

technical field [0001] The present invention relates to a negative thermal expansion material that contracts with temperature rise and a composite material including the negative thermal expansion material. Background technique [0002] Most substances increase in length and volume due to thermal expansion when the temperature rises. On the other hand, there are also known materials that exhibit negative thermal expansion (hereinafter, sometimes referred to as "negative thermal expansion materials") that shrink in volume when the temperature rises. It is known that a material exhibiting negative thermal expansion can suppress a change in the thermal expansion of the material due to a temperature change when used together with other materials. [0003] As materials showing negative thermal expansion, for example, β-eucryptite, zirconium tungstate (ZrW 2 o 8 ), zirconium phosphate tungstate (Zr 2 WO 4 (PO 4 ) 2 ), Zn x Cd 1-x (CN) 2 , manganese nitride, bismuth nicke...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45
CPCC04B14/366C01P2004/32C01P2004/61C01P2006/12C01P2006/32C04B2103/52C04B22/008C04B35/447C04B35/62655C04B2235/3244C04B2235/3258C04B2235/5296C04B2235/5409C04B2235/5436C04B2235/5445C04B2235/549C04B2235/6567C04B2235/72C04B2235/77C04B2235/9607C01B25/45C01B25/372C01P2004/45C01P2006/11B01J2/06C01P2002/74C09C1/00C04B35/00
Inventor 深泽纯也畠透
Owner NIPPON CHECMICAL IND CO LTD