CN100500611C - Conductive negative thermal expansion ceramic - Google Patents

Conductive negative thermal expansion ceramic Download PDF

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Publication number
CN100500611C
CN100500611C CNB2006101650318A CN200610165031A CN100500611C CN 100500611 C CN100500611 C CN 100500611C CN B2006101650318 A CNB2006101650318 A CN B2006101650318A CN 200610165031 A CN200610165031 A CN 200610165031A CN 100500611 C CN100500611 C CN 100500611C
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China
Prior art keywords
ball milling
thermal expansion
hour
quenching
negative thermal
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CNB2006101650318A
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CN1974480A (en
Inventor
邢献然
李璐
孙策
刘桂荣
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Abstract

The present invention relates to inorganic non-metal material, and is especially conductive ceramic with use range of 400-700 deg.c and negative heat expansion coefficient. It is high temperature solid phase prepared Zr1-xYbxW2O8 ceramic, where x is 0.0-0.1. Its preparation process includes the following steps: preparing the initial materials including ZrO2, WO3 and Yb2O3 in the stoichiometric proportion of Zr1-xYbxW2O8, ball milling inside alcohol solution for 1-24 hr, pressing into tablet, calcining at 1100-1300 deg.c for 1-48 hr, quenching to room temperature, ball milling inside alcohol solution for 1-24 hr, pressing into tablet, sintering at 1100-1300 deg.c for 1-24 hr, and cooling. The compound of the present invention has simple preparation process, negative heat expansion coefficient in wide temperature range and conductivity increased to the semiconductor conductivity range at 400 deg.c.

Description

A kind of conductive negative thermal expansion ceramic
Technical field
The invention belongs to field of inorganic nonmetallic material, particularly a kind of that can in 400~700 ℃ of scopes, use and have a conductivity negative thermal expansion ceramic.
Background technology
The negative expansion material has very high research and actual application value, along with the volume of this class material of variation of temperature is the negative expansion characteristic.This class material use range is very wide, from daily necessities to the aerospace field.At present, a lot of materials are in the news and have the negative expansion performance, as: cubical negative thermal expansion material ZrW 2O 8, having isotropic negative expansion performance, negative thermal expansion coefficient is-8.7 * 10 -6K -1The Sc of orthohormbic structure 2(WO 4) 3, negative thermal expansion coefficient is-6.5 * 10 -6K -1The CuLaO of delafossite structure 2Also be the material with negative expansion behavior, average negative thermal expansion coefficient is-6.4 * 1 -6K -1YbGaGe has the zero thermal expansion performance.But these reports all only concentrate on material and have the negative expansion performance, and whether material is had other performance simultaneously, do not see relevant report so far.At present, for the field of precision instruments of high-temperature electric conduction, the precision instrument that adopts common electro-conductive material preparation at high temperature can cause that instrument is unbalance owing to the material expansible changes because the coefficient of expansion separately is not complementary, both reduce the work-ing life of instrument, influenced the precision of instrument again.So if a kind of material also has some other performance when possessing the negative expansion performance, its range of application will increase greatly, possess higher exploitation and be worth.
Summary of the invention
The object of the invention is to study a kind of negative expansion performance that both had, and has the functional materials of conductivity again in the certain temperature interval.
A kind of conductive negative thermal expansion ceramic is characterized in that utilizing high temperature solid-state method to prepare Zr 1-xYb xW 2O 8(0.0≤x≤0.1) powder, initial feed is ZrO 2, WO 3And Yb 2O 3According to Zr 1-xYb xW 2O 8Take by weighing the ZrO that meets chemical dosage ratio 2, WO 3And Yb 2O 3Sample after weighing ball milling in ethanolic soln made its thorough mixing in 1~24 hour, pressed by powder behind the ball milling is in blocks, in 1100~1300 ℃ of temperature ranges, calcined 1~48 hour, quenching is to room temperature, and ball milling is after 1~24 hour in ethanolic soln for the sample behind the quenching, and compacting in flakes, sintering is 1~24 hour in 1100~1300 ℃ of temperature ranges, and cooled sample is the negative expansion material Zr with conductivity 1-xYb xW 2O 8
The compounds of this invention Zr 0.90Yb 0.10W 2O 8Synthetic method is simple and easy, has the negative expansion characteristic in very wide temperature range, and these chemicals are increased between semiconductor region 400 ℃ of specific conductivity simultaneously.
Description of drawings
Fig. 1 is ZrW 2O 8Compounds X RD collection of illustrative plates.
Fig. 2 is 300 ℃ of ZrW 2O 8The compound specific conductivity.
Fig. 3 is 400 ℃ of ZrW 2O 8The compound specific conductivity.
Fig. 4 is 500 ℃ of ZrW 2O 8The compound specific conductivity.
Fig. 5 is 600 ℃ of ZrW 2O 8The compound specific conductivity
Fig. 6 is 700 ℃ of ZrW 2O 8The compound specific conductivity
Fig. 7 is Zr 0.90Yb 0.10W 2O 8Compounds X RD collection of illustrative plates
Fig. 8 is Zr 0.90Yb 0.10W 2O 8The relation of compound cell parameter and temperature
Fig. 9 is 300 ℃ of Zr 0.90Yb 0.10W 2O 8The compound specific conductivity
Figure 10 is 400 ℃ of Zr 0.90Yb 0.10W 2O 8The compound specific conductivity
Figure 11 is 500 ℃ of Zr 0.90Yb 0.10W 2O 8The compound specific conductivity
Figure 12 is 600 ℃ of Zr 0.90Yb 0.10W 2O 8The compound specific conductivity
700 ℃ of Zr of Figure 13 0.90Yb 0.10W 2O 8The compound specific conductivity
Embodiment
Embodiment one:
Utilize the synthetic ZrW of this invention 2O 8Take by weighing 2.0995 gram ZrO 2, 7.9005 the gram WO 3, ball milling is after 12 hours in ethanolic soln, and powder is 80 ℃ of oven dry, and compacting is in flakes, in 1200 ℃ of down calcinings 20 hours, quenching is to room temperature, sample ball milling 10 hours once more behind the quenching, and compacting is in flakes, 1200 ℃ of sintering 1 hour, quenching promptly obtained negative expansion material ZrW to room temperature 2O 8
Fig. 1 illustrates ZrW 2O 8Compound is single phase.Fig. 2~Fig. 6 is this compound specific conductivity and variation of temperature relation, and the specific conductivity temperature influence is bigger as we know from the figure, and temperature is high more, and the specific conductivity of this compound is high more.
Embodiment two:
Utilize the synthetic Zr of this invention 0.90Yb 0.10W 2O 8Take by weighing 1.8903 gram ZrO 2, 7.9036 the gram WO 3And 0.1925 the gram Yb 2O 3, ball milling after 12 hours in ethanolic soln, powder be 80 ℃ of oven dry, compacting in flakes, in 1200 ℃ of calcinings 20 hours down, sample ball milling 10 hours once more behind the quenching, compacting in flakes, 1200 ℃ of sintering 1 hour, quenching promptly obtained negative expansion material Zr to room temperature 0.90Yb 0.10W 2O 8
Fig. 7 illustrates Zr 0.90Yb 0.10W 2O 8Compound is single phase.Fig. 8 is this compound cell parameter and variation of temperature relation, from then among the figure as can be seen unit-cell volume be not acted upon by temperature changes substantially, have the negative expansion material characteristics.Fig. 9~Figure 13 is this compound specific conductivity and variation of temperature relation, can know from figure, and temperature is high more, and the specific conductivity of this compound is high more.

Claims (1)

1. a conductive negative thermal expansion ceramic is characterized in that utilizing high temperature solid-state method to prepare Zr 0.90Yb 0.10W 2O 8, initial feed is ZrO 2, WO 3And Yb 2O 3According to Zr 0.90Yb 0.10W 2O 8Take by weighing the ZrO that meets chemical dosage ratio 2, WO 3And Yb 2O 3Sample after weighing ball milling 1~24 hour in ethanolic soln, pressed by powder behind the ball milling is in blocks, in 1100~1300 ℃ of temperature ranges, calcined 1~48 hour, quenching is to room temperature, and ball milling is after 1~24 hour in ethanolic soln for the product behind the quenching, and compacting in flakes, sintering is 1~24 hour in 1100~1300 ℃ of temperature ranges, and cooled sample is the negative thermal expansion material Zr with conductivity 0.90Yb 0.10W 2O 8
CNB2006101650318A 2006-12-12 2006-12-12 Conductive negative thermal expansion ceramic Expired - Fee Related CN100500611C (en)

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Application Number Priority Date Filing Date Title
CNB2006101650318A CN100500611C (en) 2006-12-12 2006-12-12 Conductive negative thermal expansion ceramic

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Application Number Priority Date Filing Date Title
CNB2006101650318A CN100500611C (en) 2006-12-12 2006-12-12 Conductive negative thermal expansion ceramic

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CN1974480A CN1974480A (en) 2007-06-06
CN100500611C true CN100500611C (en) 2009-06-17

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Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110591706A (en) * 2019-09-12 2019-12-20 天津大学 Rare earth ion doped cubic phase zirconium tungstate up-conversion nanocrystal and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
固相法合成负热膨胀性粉体ZrW2O8. 程晓农等.江苏大学学报,第26卷第4期. 2005
固相法合成负热膨胀性粉体ZrW2O8. 程晓农等.江苏大学学报,第26卷第4期. 2005 *

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