2-substituted cubic-phase zirconium tungstate solid solution temperature-sensitive dispersion compensation porcelain body and preparing method therefor

A technology of dispersion compensation and ceramic body, which is applied in the fields of double-substituted zirconium tungstate ceramic body and its preparation, heat-shrinkable ceramic body and its preparation, and can solve the problem of component deviation from stoichiometric ratio, complex process, and poor compactness of ceramic body and other problems to achieve the effect of reducing the pressure and simplifying the operation steps

Inactive Publication Date: 2006-10-25
BEIJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high solubility of Zr and Mo in strongly acidic solution, the above method prepares Mo-rich (Zr 1-x A x )(W 2-y Mo y )O 8-δ The solid solution is easy to cause the components to deviate from the stoichiometric ratio, resulting in the second phase compound, which complicates the process
The obtained cubic phase (Zr 1-x A x )(W 2-y Mo y )O 8-δ After solid solution dry pressing, the green body must be densified by means of the second high-temperature calcination, and the compactness of the obtained ceramic body is not good.

Method used

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  • 2-substituted cubic-phase zirconium tungstate solid solution temperature-sensitive dispersion compensation porcelain body and preparing method therefor
  • 2-substituted cubic-phase zirconium tungstate solid solution temperature-sensitive dispersion compensation porcelain body and preparing method therefor
  • 2-substituted cubic-phase zirconium tungstate solid solution temperature-sensitive dispersion compensation porcelain body and preparing method therefor

Examples

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Effect test

Embodiment 1

[0046] Example 1 Zirconium tungstomolybdate ZrW 2-y Mo y o 8 (y=0-1.3) preparation of ceramic body

[0047] According to the stoichiometric ratio of the molecular formula, add ammonium paratungstate to a three-necked bottle filled with 20ml of deionized water, and stir; dissolve zirconium oxychloride and ammonium molybdate in 30ml of deionized water, and add it dropwise to ammonium paratungstate at the same time with a constant pressure funnel The solution was stirred for several hours. Dry the co-precipitation, grind it finely, and calcinate at 600°C for 3 hours to obtain the precursor, take out the precursor and grind it, the characteristic X-ray diffraction of the obtained precursor is as follows: figure 2 shown. Weigh about 0.6g of the precursor and put it into a stainless steel mold coated with lubricant, first use a pressure of 2MPa, and then use a pressure of 4MPa for a few minutes to uniaxially dry press it into a green body. First put the green body in a platinum...

Embodiment 2

[0048] Example 2 Zr 0.96 Yb 0.04 wxya 7.98 Preparation of Ceramic Body

[0049] Add 5.2095g of ammonium paratungstate into a three-necked bottle filled with 20ml of deionized water, stir; weigh 0.1576g of Yb 2 o 3 Put into 5ml of concentrated nitric acid and heat to dissolve; 6.1273g of zirconium oxychloride and 3.5466g of ammonium molybdate were dissolved in 30ml of deionized water respectively, and were added dropwise to the ammonium paratungstate solution at the same time with a constant pressure funnel, and then the prepared Yb(NO 3 ) 3 Add dropwise to the coprecipitate and continue stirring for several hours. The co-precipitation was dried, ground into fine powder, and calcined at 600° C. for 3 hours to obtain the precursor. Take out the precursor and grind it, weigh about 0.6g and put it into a stainless steel mold coated with lubricant, first use a pressure of 2MPa, and then use a pressure of 4MPa for a few minutes to uniaxially dry press it into a green body. Fi...

Embodiment 3

[0050] Example 3 moisture resistance

[0051] Soak the three ceramic bodies prepared in Example 2 in deionized water for 120 hours, take them out, dry the water with paper, and calculate the water absorption rate of the ceramic bodies to be 2.8% according to the mass before and after soaking. After immersion, no microcracks appeared in the ceramic body, indicating that the ceramic body had good moisture resistance. Use TMA to raise the temperature from 25°C to 300°C at a rate of 3°C / min and then drop it to 50°C at the same rate to measure the thermal expansion and thermal hysteresis of the ceramic body before and after immersion ( Figure 8 a, b are the thermal expansion and thermal hysteresis curves of the ceramic body before and after soaking respectively), and the expansion coefficients are -4.2×10 -6 / °C and -4.5×10 -6 / °C.

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Abstract

This invention relates to one kind of disubstituted cube zirconium tungstate solid solution temperature sensitive dispersion compensation thermal shrinking ceramic body and its preparation method. Binding sol-gel method and high temperature solid phase method are used in this invention to make solid solution ceramic, its chemical formula is (Zr1-xAx)(W2-yMoy)O8-delta, and A equals to Yb,Er,Dy,Eu,Ce,Ga,Mn,Cu,Zn etc. X equals to 0-0.1, y equals to 0-1.3, delta equals to 0-0.1. The ceramic body with basic structure cube phase ZrW208 has linear thermal shrinking character of isotropy, good damp resistance character, its thermal lag character is low, thermoshock resistance is good, which can be used as no heat source temperature sensitive dispersion compensation compact ceramic basal body of Prague optical grating of adjustable minus thermal expansion coefficient.Its preparation technique is simple, manufacturing condition is easy to control, and material thermal shrinking and other physical property can be controlled by adjusting its components.

Description

technical field [0001] The invention relates to a heat-shrinkable ceramic body and a preparation method thereof, in particular to a double-substituted zirconium tungstate ceramic body and a preparation method thereof which shrink linearly within a temperature range from room temperature to 600°C. By adopting the method provided by the invention, a series of heat-shrinkable ceramic bodies with density and controllable porosity within a certain range can be prepared. It can be used as the ceramic substrate of the temperature-sensitive dispersion compensation Bragg optical fiber grating device of the optical filter, and belongs to the technical field of electronic device materials or photoelectric device materials. Background technique [0002] Fiber Bragg Grating (Fiber Bragg Grating, FBG) is currently the best narrow-band optical filter, used in almost every field of modern optoelectronic communication and precision optical instruments. Eliminate the FBG peak reflection wave...

Claims

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Application Information

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IPC IPC(8): C04B35/495C04B35/622
Inventor 赵新华赵瑞奇
Owner BEIJING NORMAL UNIVERSITY
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