CN114408968A - Rare earth stabilized zirconia nano powder and preparation method thereof - Google Patents
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Abstract
The invention provides rare earth stabilized zirconia nano powder and a preparation method thereof, belonging to the technical field of powder materials. The preparation method of the rare earth stabilized zirconia nano powder comprises the following steps: mixing and dissolving rare earth salt, zirconium salt and water to obtain precursor solution; drying the precursor solution to obtain a crystalline salt; ball-milling the crystalline salt, the dispersant and the alkali metal reactant to obtain a paste; adding water into the paste, and performing ultrasonic washing and suction filtration to obtain a slurry cake; drying the slurry cake to obtain precursor powder; and calcining the precursor powder to obtain the rare earth stabilized zirconia nano powder. The preparation method provided by the invention has the advantages of high cost benefit, easy operation and no pollution, and can effectively control the soft agglomeration among crystal grains, effectively relieve the phenomenon of overlarge crystal grains, and ensure that the prepared rare earth stabilized zirconia nano powder has the characteristics of uniform granularity, high dispersibility and high crystallinity.
Description
Technical Field
The invention relates to the technical field of powder materials, in particular to rare earth stabilized zirconia nano powder and a preparation method thereof.
Background
Rare earth stabilized zirconia (e.g., yttria stabilized zirconia, YSZ; scandium stabilized zirconia, SSZ) is an excellent oxygen ion conductor and is widely used in the fields of solid oxide fuel cells, oxygen sensors, oxygen separation membranes, and the like. In addition, rare earth stabilized zirconia is an important structural ceramic. In the above applications, the rare earth stabilized zirconia needs to be sintered into dense ceramics, and the nano powder is the key to improve the sintering activity of ceramics. Therefore, the ideal high-activity rare earth stabilized zirconia powder should have the characteristics of small particle size (nanometer level), narrow particle size distribution range, small agglomeration and the like.
The preparation method of the zirconia-based nano powder mainly comprises a solid phase method and a liquid phase method. The solid phase method has the advantages of simple process, high yield and low cost, but the crystal size is larger and uneven, and impurities are easily introduced in the ball milling process. The liquid phase method has the advantages of controllable grain size and high product purity. Common liquid phase methods include chemical coprecipitation, hydrothermal, sol-gel, combustion synthesis, and the like. The patent (application number: 201210580238.7) adopts a chemical coprecipitation method to prepare scandia-stabilized zirconia nano powder; the patent (application number: 200410097794.4) adopts a microwave hydrothermal method to prepare nano yttrium oxide stabilized zirconia powder; the patent (application number: 201510946404.4) adopts a sol-gel method to prepare yttria-stabilized zirconia powder with smaller grain diameter and better uniformity; the patent (application number: 201611191314.X) adopts a hydrothermal method to prepare spherical yttrium-stabilized zirconia nano-powder with uniform size; the patent (application number: 201310473256.X) adopts a combustion method to synthesize the yttria-stabilized zirconia nano-powder with high specific surface area.
However, the liquid phase method also has some problems. For example: the chemical coprecipitation method has the problem that the powder granularity, crystal form, yield and purity are unstable along with the change of solution concentration; the hydrothermal method has the problems of difficult particle dispersion, complex equipment and easy corrosion; the sol-gel method has the problems of high production cost and difficult control of the colloidal particle forming process; the combustion method has the problems of high equipment requirement, low yield and environmental pollution caused by tail gas.
Therefore, there is a need to develop a simple, easy, green and environmentally friendly method for preparing rare earth stabilized zirconia nanopowder.
Disclosure of Invention
In view of the above, the present invention aims to provide a rare earth stabilized zirconia nano-powder and a preparation method thereof. The preparation method can effectively control the soft agglomeration among the crystal grains, effectively relieve the phenomenon of overlarge crystal grains, and ensure that the prepared rare earth stabilized zirconia nano powder has the characteristics of uniform granularity, high dispersibility and high crystallinity.
The invention provides a preparation method of rare earth stabilized zirconia nano powder, which comprises the following steps:
mixing and dissolving rare earth salt, zirconium salt and water to obtain precursor solution;
drying the precursor solution to obtain a crystalline salt;
ball-milling the crystalline salt, the dispersant and the alkali metal reactant to obtain a paste;
adding water into the paste, and performing ultrasonic washing and suction filtration to obtain a slurry cake;
drying the slurry cake to obtain precursor powder;
and calcining the precursor powder to obtain the rare earth stabilized zirconia nano powder.
Preferably, the molar ratio of the rare earth element to the zirconium element in the rare earth salt and the zirconium salt is 1: 4-25.
Preferably, the rare earth salt is a yttrium salt or a scandium salt, and the yttrium salt comprises one or more of hydrated yttrium nitrate, hydrated yttrium sulfate and hydrated yttrium chloride; the scandium salt includes one or more of hydrated scandium nitrate, hydrated scandium sulfate, and hydrated scandium chloride.
Preferably, the zirconium salt comprises one or more of hydrous zirconium nitrate, hydrous zirconium sulfate and hydrous zirconium oxychloride.
Preferably, the drying temperature of the precursor liquid is 100-140 ℃.
Preferably, the dispersing agent comprises polyethylene glycol or tween, and the addition amount of the dispersing agent is 0.5-3 wt% of the crystalline salt.
Preferably, the alkali metal reactant comprises one or more of sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate, and the addition amount of the alkali metal reactant is 1-3 times of the amount of the zirconium element substance.
Preferably, the pulp cake is dried by adopting a microwave drying process, and the temperature of the microwave drying process is 100-140 ℃.
Preferably, the temperature rise rate of the calcination is 2-10 ℃/min, the temperature is 600-900 ℃, and the time is 1-5 hours.
The invention provides the rare earth stabilized zirconia nano powder prepared by the preparation method.
A preparation method of rare earth stabilized zirconia nano powder comprises the following steps: mixing and dissolving rare earth salt, zirconium salt and water to obtain precursor solution; drying the precursor solution to obtain a crystalline salt; ball-milling the crystalline salt, the dispersant and the alkali metal reactant to obtain a paste; adding water into the paste, and performing ultrasonic washing and suction filtration to obtain a slurry cake; drying the slurry cake to obtain precursor powder; and calcining the precursor powder to obtain the rare earth stabilized zirconia nano powder. The traditional room temperature solid phase method is to mix various nitrates, add a dispersant and an alkali metal reactant hydroxide or carbonate, and react by ball milling, which cannot ensure highly uniform distribution of each element. The invention adopts an improved room temperature solid phase method, firstly rare earth salt and zirconium salt are dissolved, then crystal salt is obtained by drying, uniform mixing of various elements in molecular level is realized, the crystal salt and alkali metal reactant hydroxide or carbonate are generated into water-insoluble precipitate in the process of ball milling, required powder is obtained after washing and calcining, and the washed solution is nitrate, chloride and the like of the alkali metal reactant, and can be crystallized and reused. The method provided by the invention has the advantages of simple process, no pollution, no need of complex equipment and superiority to the solution method; and the particle size is fine and uniform, the components are uniform, the performance is good, and the method is superior to a solid phase method. Meanwhile, the preparation method provided by the invention can effectively control the soft agglomeration among the crystal grains, effectively relieve the phenomenon of overlarge crystal grains, and ensure that the prepared rare earth stabilized zirconia nano powder has the characteristics of uniform granularity, high dispersibility and high crystallinity.
Drawings
FIG. 1 is an X-ray diffraction pattern of yttrium-stabilized zirconia nanopowder prepared in example 1 of the present invention;
FIG. 2 is an X-ray diffraction pattern of the scandium-stabilized zirconia nanopowder prepared in example 5 of the present invention;
FIG. 3 is a scanning electron microscope image of yttrium-stabilized zirconia nanopowder prepared in example 1 of the present invention.
Detailed Description
The invention provides a preparation method of rare earth stabilized zirconia nano powder, which comprises the following steps:
mixing and dissolving rare earth salt, zirconium salt and water to obtain precursor solution;
drying the precursor solution to obtain a crystalline salt;
ball-milling the crystalline salt, the dispersant and the alkali metal reactant to obtain a paste;
adding water into the paste, and performing ultrasonic washing and suction filtration to obtain a slurry cake;
drying the slurry cake to obtain precursor powder;
and calcining the precursor powder to obtain the rare earth stabilized zirconia nano powder.
The invention mixes and dissolves rare earth salt, zirconium salt and water to obtain precursor solution.
In the invention, the molar ratio of the rare earth element to the zirconium element in the rare earth salt and the zirconium salt is preferably 1: 4-25; the rare earth salt preferably comprises yttrium salt or scandium salt, and the yttrium salt preferably comprises one or more of hydrated yttrium nitrate, hydrated yttrium sulfate and hydrated yttrium chloride; the scandium salt preferably comprises one or more of hydrated scandium nitrate, hydrated scandium sulfate and hydrated scandium chloride; the zirconium salt preferably comprises one or more of hydrous zirconium nitrate, hydrous zirconium sulfate and hydrous zirconium oxychloride. The source of the rare earth salt and the zirconium salt is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used.
In the present invention, the water is preferably deionized water, and the mixing manner of the present invention is not particularly limited, and the rare earth salt and the zirconium salt can be uniformly dissolved in the deionized water, for example, by stirring.
After the precursor liquid is obtained, the invention dries the precursor liquid to obtain the crystal salt.
In the present invention, the temperature for drying the precursor solution is preferably 100 to 140 ℃, more preferably 120 ℃, and the time for drying the precursor solution is not particularly limited, and the crystalline salt may be obtained.
After the crystalline salt is obtained, the invention ball-mills the crystalline salt, the dispersant and the alkali metal reactant to obtain a paste.
In the invention, the dispersing agent preferably comprises polyethylene glycol or tween, and the addition amount of the dispersing agent is preferably 0.5-3 wt% of the crystalline salt, and more preferably 1 wt%; the alkali metal reactant preferably comprises one or more of sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate, and the addition amount of the alkali metal reactant is preferably 1-3 times, more preferably 2 times of the amount of the zirconium element substance. The sources of the dispersant and the alkali metal reactant are not particularly limited in the present invention, and commercially available products well known to those skilled in the art may be used. In the invention, the dispersing agent can ensure that the crystal grains are uniformly nucleated in the ball milling process and inhibit the crystal grains from growing; the alkali metal reactant reacts with the rare earth element in the crystalline salt to generate insoluble salt with uniform components.
In the invention, the ball milling is preferably carried out in a planetary ball mill, the medium for ball milling is preferably zirconia balls, and the time for ball milling is preferably 45 minutes.
After the paste is obtained, water is added into the paste, and the paste is subjected to ultrasonic washing and suction filtration to obtain a pulp cake.
In the present invention, the power of the ultrasound is preferably 90W, the temperature of the ultrasound is preferably room temperature, and the time of the ultrasound is preferably 30 minutes. The ultrasonic can improve the washing efficiency of the residues on the surface of the precursor powder and inhibit the agglomeration of the precursor powder.
The invention has no special limitation on the suction filtration mode and process, and the filtrate is subjected to solid-liquid separation by adopting a mode well known in the field to obtain a slurry cake.
According to the invention, deionized water is preferably added into the paste, and the steps of ultrasonic washing and suction filtration are repeated for 2-5 times until the washing liquid is neutral, so that the pulp cake is obtained.
After the slurry cake is obtained, the slurry cake is dried to obtain precursor powder.
In the invention, the pulp cake is preferably dried by adopting a microwave drying process, and the temperature of the microwave drying is preferably 100-140 ℃, and more preferably 120 ℃.
After the precursor powder is obtained, the invention preferentially calcines the precursor powder to obtain the rare earth stabilized zirconia nano powder.
In the invention, the heating rate of the calcination is preferably 2-10 ℃/min, more preferably 6 ℃/min, the temperature is 600-900 ℃, more preferably 750 ℃, and the time is 1-5 hours, more preferably 3 hours.
In order to further illustrate the present invention, the rare earth stabilized zirconia nanopowder and the preparation method thereof provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
A preparation method of rare earth stabilized zirconia nano powder comprises the following steps:
(1) weighing 10.46g of yttrium nitrate hexahydrate and 67.40g of zirconium nitrate pentahydrate, dissolving the yttrium nitrate hexahydrate and the zirconium nitrate pentahydrate in deionized water, and stirring to obtain a precursor solution;
(2) drying the precursor solution at 100 ℃ to obtain a crystalline salt;
(3) adding 1 wt% of polyethylene glycol serving as a dispersing agent into the crystallized salt to react with 33.28g of sodium carbonate, and performing ball milling to obtain paste;
(4) adding deionized water into the paste, and repeatedly performing ultrasonic washing and suction filtration until the washing liquid is neutral to obtain a pulp cake;
(5) drying the pulp cake at 100 ℃ by adopting a microwave drying process to obtain precursor powder;
(6) the temperature was maintained at 900 ℃ for 1 hour at a temperature rise rate of 10 ℃/min to obtain 21.53g of yttrium-stabilized zirconia nanopowder (theoretical yield 22.43g, yield 96%).
The XRD characterization of the product obtained above, as shown in fig. 1, observed that the powder is stable in cubic system without the existence of impurity phase, and as shown in fig. 3, observed that the product is spherical nano-powder with uniform grain distribution and high dispersibility by scanning electron microscopy.
Example 2
A preparation method of rare earth stabilized zirconia nano powder comprises the following steps:
(1) weighing 10.46g of yttrium nitrate hexahydrate and 50.59g of zirconium oxychloride octahydrate, dissolving the yttrium nitrate hexahydrate and the zirconium oxychloride octahydrate in deionized water, and stirring to obtain a precursor solution;
(2) drying the precursor solution at 140 ℃ to obtain a crystalline salt;
(3) adding 0.5 wt% of tween-80 serving as a dispersing agent and 33.28g of sodium carbonate into the crystallized salt to react, and performing ball milling to obtain paste;
(4) adding deionized water into the paste, and repeatedly performing ultrasonic washing and suction filtration until the washing liquid is neutral to obtain a pulp cake;
(5) drying the pulp cake at 100 ℃ by adopting a microwave drying process to obtain precursor powder;
(6) the temperature was maintained at 600 ℃ for 5 hours at a temperature rise rate of 2 ℃/min to obtain 21.08g of yttrium-stabilized zirconia nanopowder (theoretical yield 22.43g, yield 94%).
The XRD representation of the prepared product shows that the powder is stabilized in a cubic crystal system and has no impurity phase, and the product is spherical nano powder with uniform grain distribution and high dispersibility through the observation of a scanning electron microscope.
Example 3
A preparation method of rare earth stabilized zirconia nano powder comprises the following steps:
(1) weighing 12.72g of yttrium sulfate octahydrate and 50.59g of zirconium oxychloride octahydrate, dissolving the yttrium sulfate octahydrate and the zirconium oxychloride octahydrate in deionized water, and stirring to obtain a precursor solution;
(2) drying the precursor solution at 100 ℃ to obtain a crystalline salt;
(3) adding 1.5 wt% of polyethylene glycol serving as a dispersing agent into the crystallized salt to react with 17.62g of potassium hydroxide, and performing ball milling to obtain paste;
(4) adding deionized water into the paste, and repeatedly performing ultrasonic washing and suction filtration until the washing liquid is neutral to obtain a pulp cake;
(5) drying the pulp cake at 140 ℃ by adopting a microwave drying process to obtain precursor powder;
(6) the temperature was maintained at 600 ℃ for 5 hours at a temperature rise rate of 10 ℃/min to obtain 21.31g of yttrium-stabilized zirconia nanopowder (theoretical yield 22.43g, yield 95%).
The XRD representation of the prepared product shows that the powder is stabilized in a cubic crystal system and has no impurity phase, and the product is spherical nano powder with uniform grain distribution and high dispersibility through the observation of a scanning electron microscope.
Example 4
A preparation method of rare earth stabilized zirconia nano powder comprises the following steps:
(1) weighing 8.28g of yttrium chloride hexahydrate and 55.80g of zirconium sulfate tetrahydrate, dissolving the yttrium chloride hexahydrate and the zirconium sulfate tetrahydrate in deionized water, and stirring to obtain a precursor solution;
(2) drying the precursor solution at 100 ℃ to obtain a crystalline salt;
(3) adding 1 wt% of polyethylene glycol serving as a dispersing agent into the crystallized salt to react with 15.70g of sodium hydroxide, and performing ball milling to obtain paste;
(4) adding deionized water into the paste, and repeatedly performing ultrasonic washing and suction filtration until the washing liquid is neutral to obtain a pulp cake;
(5) drying the pulp cake at 100 ℃ by adopting a microwave drying process to obtain precursor powder;
(6) the temperature was maintained at 900 ℃ for 1 hour at a temperature rise rate of 10 ℃/min to obtain 21.76g of yttrium-stabilized zirconia nanopowder (theoretical yield 22.43g, yield 97%).
The XRD representation of the prepared product shows that the powder is stabilized in a cubic crystal system and has no impurity phase, and the product is spherical nano powder with uniform grain distribution and high dispersibility through the observation of a scanning electron microscope.
Example 5
A preparation method of rare earth stabilized zirconia nano powder comprises the following steps:
(1) weighing 5.19g of scandium chloride hexahydrate and 31.99g of zirconium sulfate tetrahydrate, dissolving the scandium chloride hexahydrate and the zirconium sulfate tetrahydrate in deionized water, and stirring to obtain a precursor solution;
(2) drying the precursor solution at 100 ℃ to obtain a crystalline salt;
(3) adding 0.5 wt% of tween-80 serving as a dispersing agent and 24.87g of potassium carbonate into the crystalline salt to react, and performing ball milling to obtain paste;
(4) adding deionized water into the paste, and repeatedly performing ultrasonic washing and suction filtration until the washing liquid is neutral to obtain a pulp cake;
(5) drying the pulp cake at 100 ℃ by adopting a microwave drying process to obtain precursor powder;
(6) the temperature was maintained at 900 ℃ for 1 hour at a heating rate of 10 ℃/min to obtain 13.56g of scandium-stabilized zirconia nanopowder (theoretical yield 13.84g, yield 98%).
The XRD characterization of the product obtained above, as shown in fig. 2, observed that the powder is stable in cubic system without impurity phase, and the product is a spherical nano powder with uniform grain distribution and high dispersibility observed by scanning electron microscope.
Example 6
A preparation method of rare earth stabilized zirconia nano powder comprises the following steps:
(1) weighing 6.78g of scandium nitrate hexahydrate and 29g of zirconium oxychloride octahydrate, dissolving the scandium nitrate hexahydrate and the zirconium oxychloride octahydrate in deionized water, and stirring to obtain a precursor solution;
(2) drying the precursor solution at 140 ℃ to obtain a crystalline salt;
(3) adding 2.5 wt% of polyethylene glycol serving as a dispersing agent into the crystallized salt to react with 7.2g of sodium hydroxide, and performing ball milling to obtain paste;
(4) adding deionized water into the paste, and repeatedly performing ultrasonic washing and suction filtration until the washing liquid is neutral to obtain a pulp cake;
(5) drying the pulp cake at 100 ℃ by adopting a microwave drying process to obtain precursor powder;
(6) the temperature was maintained at 600 ℃ for 5 hours at a heating rate of 10 ℃/min to obtain 13.15g of scandium-stabilized zirconia nanopowder (theoretical yield 13.84g, yield 95%).
The XRD representation of the prepared product shows that the powder is stabilized in a cubic crystal system and has no impurity phase, and the product is spherical nano powder with uniform grain distribution and high dispersibility through the observation of a scanning electron microscope.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (10)
1. A preparation method of rare earth stabilized zirconia nano powder is characterized by comprising the following steps:
mixing and dissolving rare earth salt, zirconium salt and water to obtain precursor solution;
drying the precursor solution to obtain a crystalline salt;
ball-milling the crystalline salt, the dispersant and the alkali metal reactant to obtain a paste;
adding water into the paste, and performing ultrasonic washing and suction filtration to obtain a slurry cake;
drying the slurry cake to obtain precursor powder;
and calcining the precursor powder to obtain the rare earth stabilized zirconia nano powder.
2. The preparation method according to claim 1, wherein the molar ratio of the rare earth element to the zirconium element in the rare earth salt and the zirconium salt is 1: 4-25.
3. The method of claim 1 or 2, wherein the rare earth salt comprises a yttrium salt or a scandium salt, the yttrium salt comprising one or more of hydrated yttrium nitrate, hydrated yttrium sulfate, and hydrated yttrium chloride; the scandium salt includes one or more of hydrated scandium nitrate, hydrated scandium sulfate, and hydrated scandium chloride.
4. The method of claim 1 or 2, wherein the zirconium salt comprises one or more of hydrous zirconium nitrate, hydrous zirconium sulfate, and hydrous zirconium oxychloride.
5. The method according to claim 1, wherein the precursor liquid is dried at a temperature of 100 to 140 ℃.
6. The method according to claim 1, wherein the dispersant comprises polyethylene glycol or tween, and the dispersant is added in an amount of 0.5 to 3 wt% of the crystalline salt.
7. The preparation method of claim 1, wherein the alkali metal reactant comprises one or more of sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate, and the addition amount of the alkali metal reactant is 1-3 times of the amount of the zirconium element substance.
8. The preparation method of claim 1, wherein the pulp cake is dried by a microwave drying process, and the temperature of the microwave drying process is 100-140 ℃.
9. The method according to claim 1, wherein the temperature rise rate of the calcination is 2 to 10 ℃/min, the calcination temperature is 600 to 900 ℃, and the calcination time is 1 to 5 hours.
10. The rare earth stabilized zirconia nanopowder prepared by the preparation method of any one of claims 1 to 9.
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| CN111204802A (en) * | 2020-02-12 | 2020-05-29 | 长裕控股集团有限公司 | Preparation method of black yttrium-stabilized zirconia powder |
| CN112939076A (en) * | 2021-04-16 | 2021-06-11 | 四川慧谷锆业有限公司 | Preparation method of yttrium-stabilized nano zirconia |
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| CN111204802A (en) * | 2020-02-12 | 2020-05-29 | 长裕控股集团有限公司 | Preparation method of black yttrium-stabilized zirconia powder |
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