CN111205095A - Method for preparing scandium-zirconium powder by spray pyrolysis and scandium-zirconium powder prepared by method - Google Patents
Method for preparing scandium-zirconium powder by spray pyrolysis and scandium-zirconium powder prepared by method Download PDFInfo
- Publication number
- CN111205095A CN111205095A CN202010054288.6A CN202010054288A CN111205095A CN 111205095 A CN111205095 A CN 111205095A CN 202010054288 A CN202010054288 A CN 202010054288A CN 111205095 A CN111205095 A CN 111205095A
- Authority
- CN
- China
- Prior art keywords
- scandium
- zirconium
- spray pyrolysis
- mixed solution
- zirconium powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62675—Thermal treatment of powders or mixtures thereof other than sintering characterised by the treatment temperature
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/6267—Pyrolysis, carbonisation or auto-combustion reactions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
- H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
- H01M8/1253—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides the electrolyte containing zirconium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Thermal Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Composite Materials (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a method for preparing scandium-zirconium powder through spray pyrolysis and scandium-zirconium powder prepared by the method. The method comprises the following steps: mixing the scandium-containing solution and the zirconium-containing solution to obtain a scandium-zirconium mixed solution; and carrying out spray pyrolysis on the scandium-zirconium mixed solution to obtain scandium-zirconium powder. The scandium-zirconium powder is prepared by adopting a spray pyrolysis method, a scandium-zirconium mixed solution is atomized into fine droplets, the fine droplets are carried into a high-temperature reaction furnace through carrier gas flow, and the droplets are sequentially subjected to the steps of solvent evaporation, solute precipitation, drying, metal salt thermal decomposition, sintering forming and the like in a short time after entering the reaction furnace, so that powder particles are finally formed. The whole process is completed quickly, the probability of collision of particles in a hearth is very small, and the collision time is short, so that the agglomeration phenomenon can be effectively reduced, and the obtained scandium-zirconium powder particles are fine, uniform in composition and good in dispersity. Meanwhile, the method has the advantages of controllable particle composition of products, continuous production, simple operation and lower raw material cost.
Description
Technical Field
The invention relates to the technical field of solid electrolyte materials, in particular to a method for preparing scandium-zirconium powder through spray pyrolysis and the scandium-zirconium powder prepared through the method.
Background
Solid Oxide Fuel Cells (SOFC) are an efficient and clean energy conversion device, and electrolytes as a key component thereof are currently the focus of research. The operating temperature of the conventional yttria-stabilized zirconia (YSZ) electrolyte is generally high at 1000 ℃ or above to obtain high electric energy conversion efficiency, and such high operating temperature can cause serious problems of interface reaction, battery component failure and the like. The scandia-stabilized zirconia (scandium-zirconium powder) is an electrolyte material with the highest oxygen ion conductivity in the existing zirconium-based electrolyte, and the conductivity at 800 ℃ is about twice that of YSZ, so that the scandia-stabilized zirconia becomes a preferred medium-low temperature electrolyte. The chemical composition, morphology, size and the like of the scandium-zirconium powder directly influence the performance of the electrolyte ceramic, and the scandium-zirconium powder plays an important role in research of scandium-zirconium electrolyte ceramic materials.
At present, the preparation method of scandium-zirconium powder mainly comprises a solid-phase crushing method, a hydrothermal method, a sol-gel method, a coprecipitation method and the like. The preparation methods have different principles and different operation modes, and the obtained products have great differences in appearance and performance. The solid phase crushing method has simple process, less pollution in the production process, good filling property, low cost and easy large-scale production, but can cause the pollution of powder, and the granularity after ball milling is relatively large. The hydrothermal method has the advantages of high product purity, high crystallinity, uniform powder particle size, good sintering performance and the like, but generally has high requirements on equipment, complex operation and larger energy consumption, and is not suitable for industrialization. The sol-gel method can obtain the uniformity of the molecular level in a short time and realize the uniform doping on the molecular level, but the raw materials required by the sol-gel method are expensive, generally need to use an organic solvent, have certain toxicity to human bodies and are easy to harden. The coprecipitation method has the advantages of simple preparation process, low cost, easy industrialization and the like, but the coprecipitation method has the disadvantages that agglomeration is easy to occur in the preparation process, large particles are formed, the sintering temperature of the ceramic is high, the sintering performance is poor and the like, and the application performance of the powder is seriously influenced. Therefore, the method for preparing the superfine scandium-zirconium powder is significant.
Disclosure of Invention
The invention mainly aims to provide a method for preparing scandium-zirconium powder through spray pyrolysis and the scandium-zirconium powder prepared through the method, so as to solve the problems of overlarge particle size, uneven distribution, overhigh raw material cost, complex operation and the like in the preparation of scandium-zirconium powder in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for preparing scandium-zirconium powder by spray pyrolysis, comprising the steps of: mixing the scandium-containing solution and the zirconium-containing solution to obtain a scandium-zirconium mixed solution; and carrying out spray pyrolysis on the scandium-zirconium mixed solution to obtain scandium-zirconium powder.
Further, in the spray pyrolysis process, the power of the ultrasonic spray head is 10-30W, the flow rate of the carrier gas is 10-50L/min, and the spray pyrolysis temperature is 400-1400 ℃.
Furthermore, in the spray pyrolysis process, the power of the ultrasonic spray head is 15-23W, the flow rate of the carrier gas is 25-40L/min, and the spray pyrolysis temperature is 800-1200 ℃.
Further, the scandium-containing solution and the zirconium-containing solution are mixed to obtain a scandium-zirconium mixed solution.
Furthermore, the cation concentration in the scandium-zirconium mixed solution is 0.01-5 mol/L.
Furthermore, the cation concentration in the scandium-zirconium mixed solution is 0.5-2 mol/L.
Further, in the scandium-zirconium mixed solution, the mole number of scandium ions is 8-13% of the total mole number of scandium ions and zirconium ions.
Further, the scandium-containing solution is an aqueous solution of scandium chloride or scandium nitrate.
Further, the zirconium-containing solution is an aqueous solution of zirconium chloride, zirconium nitrate, zirconium oxychloride, or zirconium oxynitrate.
According to another aspect of the invention, the scandium-zirconium powder prepared by the method is also provided.
The scandium-zirconium powder is prepared by adopting a spray pyrolysis method, and specifically, a scandium-zirconium mixed solution is atomized into fine droplets, the fine droplets are carried into a high-temperature reaction furnace through carrier gas flow, and the droplets are sequentially subjected to the steps of solvent evaporation, solute precipitation, drying, metal salt thermal decomposition, sintering molding and the like in a short time after entering the reaction furnace, so that powder particles are finally formed. The whole process is completed quickly, the probability of collision of particles in a hearth is very small, and the collision time is short, so that the agglomeration phenomenon can be effectively reduced, and the obtained scandium-zirconium powder particles are fine, uniform in composition and good in dispersity. Meanwhile, the method has the advantages of controllable particle composition of products, continuous production, simple operation and lower raw material cost, and is very suitable for industrial large-scale application.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a schematic flow chart of a method for preparing scandium-zirconium powder by spray pyrolysis according to an embodiment of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
As described in the background art, the problems of excessive particle size, uneven distribution, excessive raw material cost, complex operation and the like exist in the preparation of scandium-zirconium powder in the prior art.
In order to solve the above problems, the present invention provides a method for preparing scandium-zirconium powder by spray pyrolysis, as shown in fig. 1, the method comprising the steps of: mixing the scandium-containing solution and the zirconium-containing solution to obtain a scandium-zirconium mixed solution; and carrying out spray pyrolysis on the scandium-zirconium mixed solution to obtain scandium-zirconium powder.
The scandium-zirconium powder is prepared by adopting a spray pyrolysis method, and specifically, a scandium-zirconium mixed solution is atomized into fine droplets, the fine droplets are carried into a high-temperature reaction furnace through carrier gas flow, and the droplets are sequentially subjected to the steps of solvent evaporation, solute precipitation, drying, metal salt thermal decomposition, sintering molding and the like in a short time after entering the reaction furnace, so that powder particles are finally formed. The whole process is completed quickly, the probability of collision of particles in a hearth is very small, and the collision time is short, so that the agglomeration phenomenon can be effectively reduced, and the obtained scandium-zirconium powder particles are fine, uniform in composition and good in dispersity. Meanwhile, the method has the advantages of controllable particle composition of products, continuous production, simple operation and lower raw material cost, and is very suitable for industrial large-scale application.
In order to achieve better spray pyrolysis effect, in a preferred embodiment, in the spray pyrolysis process, the power of the ultrasonic spray head is 10 to 30W, the flow rate of the carrier gas is 10 to 50L/min, and the spray pyrolysis temperature is 400 to 1400 ℃. More preferably, in the spray pyrolysis process, the power of the ultrasonic spray head is 15-23W, the flow rate of the carrier gas is 25-40L/min, and the spray pyrolysis temperature is 800-1200 ℃. Under the process condition, the obtained scandium-zirconium powder has better dispersibility and has larger improvement on the conductivity after sintering. The carrier gas may be air, oxygen, or the like.
In order to further improve the dispersibility of the scandium-zirconium powder and to reduce the particle size, in a preferred embodiment, the cation concentration in the scandium-zirconium mixed solution is 0.01 to 5 mol/L. Meanwhile, in order to provide good dispersibility for the scandium-zirconium powder and improve the efficiency and effect of spray pyrolysis, the cation concentration in the scandium-zirconium mixed solution is preferably 0.5 to 2 mol/L.
In a preferred embodiment, the scandium-zirconium mixed solution has a ratio of the number of moles of scandium ions to the total number of moles of scandium ions and zirconium ions of 8 to 13%. Thus, the scandium content in the scandium-zirconium powder is more suitable, and the electrical conductivity of the sintered powder is better.
The scandium-containing solution and the zirconium-containing solution described above may be of the type commonly used in coprecipitation preparation processes, and in a preferred embodiment the scandium-containing solution is an aqueous solution of scandium chloride or scandium nitrate; more preferably, the zirconium-containing solution is an aqueous solution of zirconium chloride, zirconium nitrate, zirconium oxychloride or zirconium oxynitrate. The scandium chloride, the scandium nitrate, the zirconium chloride, the zirconium nitrate, the zirconium oxychloride and the zirconyl nitrate have good solubility in water, are beneficial to improving the dispersibility of scandium ions and zirconium ions in a scandium-zirconium mixed solution, and have better promotion effect on the dispersibility and refined particle size of scandium-zirconium powder.
In another aspect of the invention, the scandium-zirconium powder prepared by the method is also provided. As mentioned earlier, the scandium-zirconium powders produced by this method have a smaller and more uniform particle size.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1:
mixing a scandium nitrate aqueous solution and a zirconium nitrate aqueous solution to obtain a scandium-zirconium mixed solution; atomizing the scandium-zirconium mixed solution into fine droplets, carrying the droplets into a high-temperature reaction furnace through carrier gas flow, and carrying out the steps of solvent evaporation, solute precipitation, drying, metal salt thermal decomposition, sintering molding and the like in sequence in a short time after the droplets enter the reaction furnace to finally form scandium-zirconium powder. Wherein the cation concentration in the scandium-zirconium mixed solution is 0.5mol/L, and the mole number of scandium ions is 8% of the total mole number of scandium ions and zirconium ions. The power of the ultrasonic spray head is 30W, the flow rate of the carrier gas is 30L/min, and the spray pyrolysis temperature is 1200 ℃.
Example 2:
mixing a scandium chloride aqueous solution and a zirconium oxychloride aqueous solution to obtain a scandium-zirconium mixed solution; atomizing the scandium-zirconium mixed solution into fine droplets, carrying the droplets into a high-temperature reaction furnace through carrier gas flow, and carrying out the steps of solvent evaporation, solute precipitation, drying, metal salt thermal decomposition, sintering molding and the like in sequence in a short time after the droplets enter the reaction furnace to finally form scandium-zirconium powder. Wherein the cation concentration in the scandium-zirconium mixed solution is 5mol/L, and the mole number of scandium ions is 10% of the total mole number of scandium ions and zirconium ions. The power of an ultrasonic spray head is 15W, the flow rate of carrier gas is 20L/min, and the spray pyrolysis temperature is 1400 ℃.
Example 3:
mixing a scandium chloride aqueous solution and a zirconium oxychloride aqueous solution to obtain a scandium-zirconium mixed solution; atomizing the scandium-zirconium mixed solution into fine droplets, carrying the droplets into a high-temperature reaction furnace through carrier gas flow, and carrying out the steps of solvent evaporation, solute precipitation, drying, metal salt thermal decomposition, sintering molding and the like in sequence in a short time after the droplets enter the reaction furnace to finally form scandium-zirconium powder. Wherein the cation concentration in the scandium-zirconium mixed solution is 2mol/L, and the mole number of scandium ions is 13% of the total mole number of scandium ions and zirconium ions. The power of the ultrasonic spray head is 10W, the flow rate of the carrier gas is 10L/min, and the spray pyrolysis temperature is 400 ℃.
Example 4:
mixing a scandium chloride aqueous solution and a zirconium oxychloride aqueous solution to obtain a scandium-zirconium mixed solution; atomizing the scandium-zirconium mixed solution into fine droplets, carrying the droplets into a high-temperature reaction furnace through carrier gas flow, and carrying out the steps of solvent evaporation, solute precipitation, drying, metal salt thermal decomposition, sintering molding and the like in sequence in a short time after the droplets enter the reaction furnace to finally form scandium-zirconium powder. Wherein the cation concentration in the scandium-zirconium mixed solution is 1mol/L, and the mole number of scandium ions is 11% of the total mole number of scandium ions and zirconium ions. The power of an ultrasonic spray head is 25W, the flow rate of carrier gas is 25L/min, and the spray pyrolysis temperature is 900 ℃.
Example 5:
mixing a scandium nitrate aqueous solution and a zirconium nitrate aqueous solution to obtain a scandium-zirconium mixed solution; atomizing the scandium-zirconium mixed solution into fine droplets, carrying the droplets into a high-temperature reaction furnace through carrier gas flow, and carrying out the steps of solvent evaporation, solute precipitation, drying, metal salt thermal decomposition, sintering molding and the like in sequence in a short time after the droplets enter the reaction furnace to finally form scandium-zirconium powder. Wherein the cation concentration in the scandium-zirconium mixed solution is 0.01mol/L, and the mole number of scandium ions is 10% of the total mole number of scandium ions and zirconium ions. The power of an ultrasonic spray head is 20W, the flow rate of carrier gas is 50L/min, and the spray pyrolysis temperature is 1000 ℃.
The agglomerated particle size of the scandia-stabilized zirconia powder prepared in examples 1 to 5 was measured by a laser particle size analyzer, and the conductivity of the scandia-stabilized zirconia electrolyte ceramic sheet (the ceramic sheet was prepared by tape casting and sintering the scandia-stabilized zirconia powder prepared in examples 1 to 5) was measured by an ac impedance spectroscopy, and the results are shown in table 1.
TABLE 1
| Group of | Agglomerate diameter d50 (. mu.m) | 800oC conductivity (μ S/cm) |
| Example 1 | 0.12 | 245 |
| Example 2 | 0.16 | 241 |
| Example 3 | 0.22 | 250 |
| Example 4 | 0.2 | 243 |
| Example 5 | 0.18 | 252 |
The invention adopts spray pyrolysis to rapidly complete the steps of atomizing raw material liquid, evaporating solvent, precipitating solute, drying, thermally decomposing metal salt, sintering and forming and the like in one step, thereby greatly shortening the process flow, and the obtained scandium-zirconium powder has fine particles, uniform composition, controllable particle composition and continuous production. Moreover, the preparation method of the scandium-zirconium powder provided by the invention has the advantages of simple process, low cost and continuous process, avoids the use of alkaline liquids such as ammonia water and the like, and is easy to realize industrial production.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing scandium-zirconium powder by spray pyrolysis, said method comprising the steps of:
mixing the scandium-containing solution and the zirconium-containing solution to obtain a scandium-zirconium mixed solution;
and carrying out spray pyrolysis on the scandium-zirconium mixed solution to obtain scandium-zirconium powder.
2. The method according to claim 1, wherein in the spray pyrolysis process, the power of an ultrasonic spray head is 10-30W, the flow rate of the carrier gas is 10-50L/min, and the temperature of the spray pyrolysis is 400-1400 ℃.
3. The method according to claim 2, wherein in the spray pyrolysis process, the power of an ultrasonic spray head is 15-23W, the flow rate of the carrier gas is 25-40L/min, and the spray pyrolysis temperature is 800-1200 ℃.
4. The method according to any one of claims 1 to 3, wherein the scandium-zirconium mixed solution is obtained by mixing the scandium-containing solution and the zirconium-containing solution.
5. The method according to any one of claims 1 to 4, wherein the cation concentration in the scandium-zirconium mixed solution is 0.01 to 5 mol/L.
6. The method according to claim 5, wherein the cation concentration in the scandium-zirconium mixed solution is 0.5-2 mol/L.
7. The method according to claim 5, wherein the mole number of scandium ions in the scandium-zirconium mixed solution is 8-13% of the total mole number of scandium ions and zirconium ions.
8. A method according to any one of claims 1 to 3, wherein said scandium-containing solution is an aqueous solution of scandium chloride or scandium nitrate.
9. A method according to any one of claims 1 to 3, wherein the zirconium-containing solution is an aqueous solution of zirconium chloride, zirconium nitrate, zirconium oxychloride or zirconium oxynitrate.
10. Scandium-zirconium powder prepared by the method according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010054288.6A CN111205095A (en) | 2020-01-17 | 2020-01-17 | Method for preparing scandium-zirconium powder by spray pyrolysis and scandium-zirconium powder prepared by method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010054288.6A CN111205095A (en) | 2020-01-17 | 2020-01-17 | Method for preparing scandium-zirconium powder by spray pyrolysis and scandium-zirconium powder prepared by method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111205095A true CN111205095A (en) | 2020-05-29 |
Family
ID=70787528
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010054288.6A Pending CN111205095A (en) | 2020-01-17 | 2020-01-17 | Method for preparing scandium-zirconium powder by spray pyrolysis and scandium-zirconium powder prepared by method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111205095A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113371682A (en) * | 2021-05-13 | 2021-09-10 | 中国恩菲工程技术有限公司 | Nano-micron spherical powder and preparation method and equipment thereof |
| CN115055067A (en) * | 2022-05-05 | 2022-09-16 | 清华大学 | Proton conduction medium-temperature fuel cell electrolyte based on flame synthesis and preparation method thereof |
| CN116454337A (en) * | 2023-06-14 | 2023-07-18 | 潮州三环（集团）股份有限公司 | Zirconia-based electrolyte and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740372A (en) * | 2005-09-21 | 2006-03-01 | 武汉理工大学 | Liquid phase plasma spraying process of preparing nanometer zirconia thermal-barrier coating |
| CN103647097A (en) * | 2013-12-20 | 2014-03-19 | 湖南稀土金属材料研究院 | Sc2O3-stabilized ZrO2-based electrolyte powder and preparation method thereof, and Sc2O3-stabilized ZrO2 electrolyte ceramic wafer prepared from powder |
| CN104081562A (en) * | 2011-12-06 | 2014-10-01 | Sk新技术株式会社 | Method for manufacturing cathode active material for lithium secondary battery |
-
2020
- 2020-01-17 CN CN202010054288.6A patent/CN111205095A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740372A (en) * | 2005-09-21 | 2006-03-01 | 武汉理工大学 | Liquid phase plasma spraying process of preparing nanometer zirconia thermal-barrier coating |
| CN104081562A (en) * | 2011-12-06 | 2014-10-01 | Sk新技术株式会社 | Method for manufacturing cathode active material for lithium secondary battery |
| CN103647097A (en) * | 2013-12-20 | 2014-03-19 | 湖南稀土金属材料研究院 | Sc2O3-stabilized ZrO2-based electrolyte powder and preparation method thereof, and Sc2O3-stabilized ZrO2 electrolyte ceramic wafer prepared from powder |
Non-Patent Citations (2)
| Title |
|---|
| DONG HYUN PECK等人: "Electrical conductivity of Scandia stabilized zirconia for membranes in solid oxide fuel cells", 《PROCEEDINGS OF THE ELECTROCHEMICAL SOCIETY》 * |
| 叶志镇: "《半导体薄膜技术与物理》", 30 September 2008, 杭州：浙江大学出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113371682A (en) * | 2021-05-13 | 2021-09-10 | 中国恩菲工程技术有限公司 | Nano-micron spherical powder and preparation method and equipment thereof |
| CN115055067A (en) * | 2022-05-05 | 2022-09-16 | 清华大学 | Proton conduction medium-temperature fuel cell electrolyte based on flame synthesis and preparation method thereof |
| CN115055067B (en) * | 2022-05-05 | 2024-02-02 | 清华大学 | Proton conduction medium-temperature fuel cell electrolyte based on flame synthesis and preparation method thereof |
| CN116454337A (en) * | 2023-06-14 | 2023-07-18 | 潮州三环（集团）股份有限公司 | Zirconia-based electrolyte and preparation method and application thereof |
| CN116454337B (en) * | 2023-06-14 | 2024-05-14 | 潮州三环（集团）股份有限公司 | Zirconia-based electrolyte and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xu et al. | Electrochemical synthesis of ammonia using a cell with a Nafion membrane and SmFe 0.7 Cu 0.3− x Ni x O 3 (x= 0− 0.3) cathode at atmospheric pressure and lower temperature | |
| CN111205095A (en) | Method for preparing scandium-zirconium powder by spray pyrolysis and scandium-zirconium powder prepared by method | |
| CN103474645B (en) | The preparation method of lithium titanate | |
| CN108963282A (en) | A kind of fuel cell carbon carried platinum-based catalyst and the preparation method and application thereof of solvent-thermal method reduction | |
| CN106315695A (en) | Strawberry like Ni-Co nano material and preparing method thereof | |
| CN107681195B (en) | Preparation method of nano garnet type solid electrolyte material | |
| CN103157461A (en) | Nanometer photocatalyst bismuth tungstate and preparation method thereof | |
| CN102617139A (en) | Preparation method for strontium titanate lanthanum based powder material | |
| CN103647097B (en) | Sc2o3stablize ZrO2base electrolyte powder body, its preparation method and Sc2o3stablize ZrO2electrolyte ceramics sheet | |
| CN101585558A (en) | The preparation method of nano-powder of cathode of solid oxide fuel cell | |
| Venkatesan et al. | Nanomaterials and films for polymer electrolyte membrane fuel cells and solid oxide cells by flame spray pyrolysis | |
| Subramania et al. | Synthesis of nano-crystalline (Ba0. 5Sr0. 5) Co0. 8Fe0. 2O3− δ cathode material by a novel sol–gel thermolysis process for IT-SOFCs | |
| JP5439959B2 (en) | Electrode for solid oxide fuel cell and cell for solid oxide fuel cell | |
| JP6449592B2 (en) | Low alkaline nickel lithium metal composite oxide powder and method for producing the same | |
| CN111205088A (en) | Method for preparing scandia-stabilized zirconia powder by hydrothermal method and scandia-stabilized zirconia powder prepared by method | |
| CN106299301B (en) | A kind of Li with excellent storage lithium performance3VO4The pattern of nano wire mutually regulates and controls method with object | |
| Lim et al. | Ceramic nanocomposites for solid oxide fuel cells | |
| CN106745261B (en) | A kind of method of synthesis of solid oxide fuel battery electrolyte material nanometer lanthanum molybdate | |
| CN107482162A (en) | High-tap density metal oxide, preparation method and lithium ion battery | |
| Chae et al. | Sr-and Mg-doped LaGaO3 powder synthesis by carbonate coprecipitation | |
| CN106602115A (en) | Preparation method of low-temperature type solid electrolyte material | |
| CN110817954A (en) | Solid electrolyte, preparation method thereof and solid oxide fuel cell | |
| Xu et al. | Low-temperature combustion synthesis and sintering of nanosized Ce0. 8Y0. 2O1. 9 powders | |
| CN211570129U (en) | Device for preparing scandium-zirconium powder by coprecipitation coupling spray pyrolysis | |
| Nesaraj et al. | Preparation and characterization of NiO based nano-ceramic composites as alternative anode materials for solid oxide fuel cells (SOFCs) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200529 |
|
| RJ01 | Rejection of invention patent application after publication |