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Multi-element negative-expansion tungstate layer coated on microcrystal ceramics and its preparing process

A technology of microcrystalline ceramics and negative expansion, which is applied in the field of multi-component tungstate negative expansion microcrystalline ceramic coatings and its preparation, can solve the problems of interfacial stress hesitation, lack of compensation effect, difficult sintering and densification, etc., and achieve reliable Compensation effect, effect of good bonding characteristics

Inactive Publication Date: 2002-12-04
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the 1970s, former Soviet scientists studied tungstate, especially the anti-cubic phase ZrW 2 o 8 The synthesis has been intensively studied, but the cubic phase ZrW 2 o 8 It is only thermodynamically stable in a narrow temperature range around 1100 °C, the preparation process conditions are quite harsh, the synthesis is difficult and not stable, and it is difficult to obtain a single pure crystal phase, so it has not been paid attention to and applied
However, it is difficult to sinter this kind of material to be dense. Although Merkel et al. have described in detail the use of various sintering aids to increase the density in the patent specification, the sintering process is complicated and difficult to control, and the formed composite negative expansion material is also prone to cracking.
In addition, the interface contact between the negative expansion substrate material and the fiber bragg grating (FBG) device is also limited to the connecting solder joints, the interface stress is easy to hesitant, and no reliable compensation effect can be obtained.

Method used

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  • Multi-element negative-expansion tungstate layer coated on microcrystal ceramics and its preparing process
  • Multi-element negative-expansion tungstate layer coated on microcrystal ceramics and its preparing process
  • Multi-element negative-expansion tungstate layer coated on microcrystal ceramics and its preparing process

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Experimental program
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Effect test

Embodiment 1

[0026] Take commercially available Y 2 O 3 Dissolve in nitric acid solution, configure to 0.1M Y(NO 3 ) 3 Solution, with commercially available ZrO(NO 3 ) 2 Configured as 1M ZrO(NO 3 ) 2 Solution, and configure 1M ammonia complex (NH 4 ) 6 H 2 W 12 O 40 As precursors, these precursors are mixed uniformly according to the atomic ratio of the metal contained in Y:Zr:W=0.1:0.9:2.0, heated in a water bath at 60~80℃ with constant stirring, and titrated 2M into the mixed precursor Acetic acid solution until a uniform colloidal precipitate containing multiple metal atoms is completely formed. After the obtained colloidal mixture is washed and dehydrated for many times, a wet gel is formed. The formed gel is spun on a thin substrate of near-zero expansion quartz glass with a thickness of 0.30~0.40mm, and is subjected to rapid heat treatment at 600°C for 5 minutes, and then multiple cycles of spun and rapid heat treatment. In one or two quartz glass The surface is deposited with a thicknes...

Embodiment 2

[0028] Commercially available AlCl 3 Configured to 0.4M AlCl 3 Solution to commercially available ZrOCl 2 ·8H 2 O configured as 1MZrOCl 2 Solution, use commercially available phosphoric acid to configure 0.5M phosphoric acid solution, and configure 1M ammonia complex (NH 4 ) 6 H 2 W 12 O 40 These precursors are mixed uniformly according to the atomic ratio of the metal contained in Al:Zr:W:P=0.04:0.96:1.96:0.04, and then heated in a water bath at 60~80℃ with constant stirring. Titrate the 2M acetic acid solution in the body until a uniform colloidal precipitate containing multiple metal atoms is completely formed. After the obtained colloidal mixture is washed and dehydrated for many times, a wet gel is formed. The gel is spun on a thin substrate of near-zero expansion quartz glass with a thickness of 0.30~0.40mm, fast heat treatment at 650℃ for 8 minutes, and then several cycles of spun and fast heat treatment, on one or two surfaces of the quartz glass It is deposited to a thick...

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Abstract

A coated layer of ceramics contains cubic-phase ZrW2O8 sosoloid microcrystal doped by 3-valence metal element, Mo, or P and non-crystal glass, phase, and is prepared through preparing wet gel of multi-element tungstate, centrifugal coating on the zero-expansion quartz glass substrate several times, and heat treating. Its advantage is negative expansion coefficient (-2.0- -0.3X10 to the power -6 / deg.C for -20-80 deg.C).

Description

Technical field: [0001] The invention relates to a negative expansion ceramic coating and a preparation method thereof, in particular to a stable multi-element tungstate negative expansion microcrystalline ceramic coating and a preparation method thereof. The ceramic coating can be used to make temperature-compensating coating materials for electronic or optical components, especially temperature-compensating negative-expansion coatings for non-temperature-sensitive fiber grating devices. Background technique: [0002] Negative expansion materials have always received attention due to their shrinking behavior when heated. Many materials with negative expansion behavior have been discovered, such as aluminosilicate Mg 2 Al 4 Si 5 O 18 , LiAlSiO 4 And zeolite, phosphate NaZr 2 (PO 4 ) 3 , Zr(V x P 2-x )O 7 Wait. The thermal expansion behavior of these materials tends to be anisotropic, that is, contraction occurs in a certain crystallographic direction, while expansion occurs in ot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/14C04B35/488C04B35/495C04B35/622
Inventor 孔向阳吴建生
Owner SHANGHAI JIAO TONG UNIV
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