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A method for rapid sintering of fully stabilized zirconia powder at low temperature and atmospheric pressure

A fully stable zirconia, rapid sintering technology, applied in the field of fine chemicals, can solve the problems of FSZ material production cost increase, long sintering cycle, etc., to ensure performance, solve densification and grain coarsening, and inhibit the growth of grains big effect

Active Publication Date: 2018-09-11
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method can realize the sintering of FSZ ceramics at a lower temperature, it should be pointed out that the sintering period of this method is too long, and usually the holding time alone is as long as more than 20h, which will lead to a substantial increase in the production cost of FSZ materials

Method used

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  • A method for rapid sintering of fully stabilized zirconia powder at low temperature and atmospheric pressure
  • A method for rapid sintering of fully stabilized zirconia powder at low temperature and atmospheric pressure
  • A method for rapid sintering of fully stabilized zirconia powder at low temperature and atmospheric pressure

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Such as figure 1 As shown, first set Y 2 o 3 Dissolve with concentrated nitric acid to form 0.2mol l -1 Stable and transparent Y(NO 3 ) 3 solution. At the same time, zirconium sulfate was dissolved in distilled water to form 0.2mol·l -1 Stable clear solution. The above two solutions are then combined according to (Y 3+ :Zr 4+ ) molar ratio of 3:97 for mixing, and adjust the pH value to 7 with ammonia water. Add a slightly excess saturated urea solution and heat to 75°C, causing the solution to completely precipitate and form a uniform and stable co-precipitation product; then, the coprecipitation product is washed, dried at 90°C and heat-treated at 600°C 2h, the precursor was obtained after natural cooling. Then the precursor was mixed with 0.6 mol·l -1 CaCl 2 -MgCl 2 Composite molten salt (CaCl 2 / MgCl 2 Molar ratio is 0.474:0.526) solution by (Ca 2+ +Mg 2+ ):Zr 4+ The example with a molar ratio of 5:95 was mixed evenly, dried and then ground and pass...

Embodiment 2

[0036] Such as figure 1 As shown, first set Y 2 o 3 Dissolve with concentrated nitric acid to form 0.2mol l -1 Stable and transparent Y(NO 3 ) 3 solution. Simultaneously ZrOCl 2 ·8H 2 O is dissolved in distilled water to form 0.2mol l -1Stable clear solution. Then the two solutions were mixed according to (Y 3+ :Zr 4+ ) molar ratio of 8:92 for mixing, and adding 4mol l -1 KOH solution, adjust the pH value to 10 to form a uniform and stable co-precipitation product; then, the co-precipitation product was washed, dried at 90°C and heat-treated at 800°C for 1h, and the precursor was obtained after natural cooling. Then the precursor was mixed with 0.6 mol·l -1 CaCl 2 -CaO composite molten salt (CaCl 2 / CaO molar ratio is 0.938:0.062) solution according to Ca 2+ :Zr 4+ The example with a molar ratio of 3:97 was mixed evenly, dried and then ground and passed through a 120-mesh sieve. It was pressed into a green body under a pressure system of 200Mpa and a holding t...

Embodiment 3

[0038] Such as figure 1 As shown, first set YC1 3 ·7H 2 O is dissolved in distilled water to form 0.2mol l -1 Stable and transparent YCl 3 solution. At the same time, zirconium sulfate was dissolved in distilled water to form 0.2mol·l -1 Stable clear solution. The above two solutions are then combined according to (Y 3+ :Zr 4+ ) in a molar ratio of 10:90, and adjust the pH value to 7 with ammonia water. Add a slightly excess saturated urea solution and heat to 75°C, causing the solution to completely precipitate and form a uniform and stable co-precipitation product; then, the coprecipitation product is washed, dried at 90°C and heat-treated at 700°C After 1.5h, the precursor was obtained after natural cooling. Then the precursor was mixed with 0.6 mol·l -1 BaCl 2 -CaCl 2 Composite molten salt (BaCl 2 / CaCl 2 Molar ratio is 0.359:0.641) solution according to (Ba 2+ +Ca 2+ ):Zr 4+ The example with a molar ratio of 3:97 was mixed evenly, dried and then ground an...

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Abstract

The invention discloses a method for rapidly sintering fully stabilized zirconia powder under low temperature and normal pressure, which belongs to the field of fine chemical engineering. The method includes the steps of zirconium salt and stabilizer mixing, coprecipitation, washing, drying, heat treatment, mixing with molten salt solution, drying, grinding, dry pressing, calcination and the like. By introducing trace molten salt into the fully stabilized zirconia powder and utilizing the molten salt to form liquid phase under low temperature, while promoting the grain boundary diffusion of the powder, the method inhibits the grain boundary migration of the powder, consequently, the contradiction between densification and grain coarsening in the process of sintering the fully stabilized zirconia powder is solved, and the normal-pressure rapid sintering of the fully stabilized zirconia powder under low temperature is realized; in addition, cations in the molten salt get into the ZrO2 crystal lattice by doping, consequently, the ZrO2 crystal form is further stabilized, and the properties of the material are further improved; the average bending strength of the obtained sintered body is greater than 450Mpa, the theoretical density is greater than 93 percent, and the grain size is between 425nm and 520nm.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and more specifically relates to a method for rapidly sintering fully stable zirconia powder at low temperature and normal pressure. Background technique [0002] Fully stabilized zirconia (FSZ) has excellent properties such as strong high-temperature oxygen ion conductivity, low thermal conductivity, and good high-temperature stability. In recent years, it has shown extensive applications in oxygen sensors, solid oxide fuel cells, and thermal barrier coatings. application prospects. However, the sintering of FSZ powder is very difficult, and it usually needs to be above 1500 °C to achieve its densification process. But a higher temperature will lead to abnormal growth of FSZ grains, which will have an adverse effect on the electrical conductivity and mechanical properties of the material. Therefore, how to solve the contradiction between densification and grain coarsening of FSZ powder du...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/48C04B35/64
CPCC04B35/48C04B35/64C04B2235/3206C04B2235/3208C04B2235/3215C04B2235/3246C04B2235/656C04B2235/77C04B2235/785C04B2235/96
Inventor 邓义群沈针
Owner JIANGXI UNIV OF SCI & TECH
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