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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 coating and its preparation, can solve the problem of interfacial stress delay, lack of compensation effect, easy cracking of complex negative expansion materials, etc. problem, to achieve reliable compensation effect and good bonding characteristics.

Inactive Publication Date: 2004-07-28
SHANGHAI JIAOTONG 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] Commercially available Y 2 o 3 Dissolved in nitric acid solution, configured as 0.1M Y(NO 3 ) 3 solution, 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 etc. as precursors, mix these precursors according to the atomic ratio of metals Y:Zr:W=0.1:0.9:2.0, mix them evenly, heat in a water bath at 60-80°C and keep stirring, and titrate 2M into the mixed precursors Acetic acid solution until a uniform colloidal precipitate containing various metal atoms is completely formed. The obtained colloidal mixture is washed, dehydrated and other steps to form a wet gel. Spray the formed gel on a thin near-zero-expansion quartz glass substrate with a thickness of 0.30-0.40mm, heat it quickly at 600°C for 5 minutes, and then cycle the gel and rapid heat treatment several times. The surface is deposited with a thickness of 300 μm, and then densified in a rapid heat treatment furnace at 110...

Embodiment 2

[0028] Commercially available AlCl 3 Configured as 0.4M AlCl 3 solution, commercially available ZrOCl 2 ·8H 2 O configured as 1MZrOCl 2 Solution, configure 0.5M phosphoric acid solution with commercially available phosphoric acid, and configure 1M ammonia complex (NH 4 ) 6 h 2 W 12 o 40 etc. as precursors, these precursors are uniformly mixed according to the atomic ratio of the metals contained in Al: Zr: W: P = 0.04: 0.96: 1.96: 0.04, heated in a water bath at 60-80 ° C and continuously stirred, and mixed with the precursor Titrate 2M acetic acid solution in vivo until a uniform colloidal precipitate containing various metal atoms is completely formed. The obtained colloidal mixture is washed, dehydrated and other steps to form a wet gel. Spray the formed gel on a thin near-zero-expansion quartz glass substrate with a thickness of 0.30-0.40mm, heat it rapidly at 650°C for 8 minutes, and then cycle the gel and rapid heat treatment several times. It is deposited to a...

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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-component tungstate negative expansion microcrystalline ceramic coating and a preparation method thereof. The ceramic coating can be used to make temperature-compensating cladding materials for electronic or optical components, especially temperature-compensating negative-expansion cladding coatings for non-temperature-sensitive optical fiber grating devices. Background technique: [0002] Negative expansion materials have attracted much attention due to their thermal shrinkage behavior. Many materials with negative expansion behavior have been found, such as the 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 often shows anisotropy, that is, shrinkage occurs along one crystallographic direction, wh...

Claims

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Application Information

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