CN110563035A - Rare earth zirconate nano powder and preparation method and application thereof - Google Patents
Rare earth zirconate nano powder and preparation method and application thereof Download PDFInfo
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- CN110563035A CN110563035A CN201910973416.4A CN201910973416A CN110563035A CN 110563035 A CN110563035 A CN 110563035A CN 201910973416 A CN201910973416 A CN 201910973416A CN 110563035 A CN110563035 A CN 110563035A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
the invention relates to the technical field of rare earth zirconate nano materials, in particular to rare earth zirconate nano powder and a preparation method and application thereof. The invention provides a preparation method of rare earth zirconate nano powder, which comprises the following steps: mixing rare earth oxide, zirconia, molten salt and absolute ethyl alcohol to obtain a mixed material; calcining the mixed material to obtain the rare earth zirconate nano powder; the molten salt comprises sodium chloride, potassium chloride and lithium chloride; the mass ratio of the sodium chloride to the potassium chloride to the lithium chloride is 1: (1-5): (1-5); the calcining temperature is 1000-1200 ℃, and the calcining time is 2-8 h. According to the description of the embodiment, the particle size of the rare earth zirconate nano-powder prepared by the preparation method is 50-200 nm.
Description
Technical Field
The invention relates to the technical field of rare earth zirconate nano materials, in particular to rare earth zirconate nano powder and a preparation method and application thereof.
Background
The rare earth zirconate material has the characteristics of high melting point, low thermal conductivity, high thermal expansion coefficient, high chemical stability, relatively low conduction temperature, excellent ionic conductivity, high radiation stability and the like, and is widely applied to various fields such as refractory materials, thermal barrier coating materials, high-temperature solid electrolyte materials, main materials for fixing actinides in nuclear waste materials and the like.
The superfine high-purity rare earth zirconate powder is the key for preparing the high-performance rare earth zirconate material. At present, the preparation method of the rare earth zirconate powder mainly comprises a high-temperature solid phase method, a hydrothermal method, a coprecipitation method, a combustion method, a sol-gel method, a molten salt method and the like. The high-temperature solid phase method is difficult to realize the uniform mixing of powder, the synthesis temperature is high, the sintering activity of the prepared powder is low, and the temperature for preparing ceramics is generally higher than 1600 ℃; batch production is difficult to realize by a hydrothermal method, a coprecipitation method, a sol-gel method and the like. The molten salt method realizes the uniform mixing of reactants on a molecular scale due to the special liquid phase reaction environment, can effectively solve the problem of overlong diffusion path of the reactants in the solid-solid reaction, and finally achieves the aim of quickly synthesizing the target product at low temperature. However, the existing molten salt system has sulfate radicals and the like, which can cause damage to the volatilization kettle equipment of the molten salt, and the melting point of the currently adopted molten salt medium is generally higher.
disclosure of Invention
The invention aims to provide rare earth zirconate nano powder and a preparation method and application thereof, the preparation method disclosed by the invention is low in synthesis temperature and small in damage to production equipment, and the particle size of the prepared rare earth zirconate nano powder is small and is within the range of 50-200 nm.
In order to achieve the above object, the present invention provides the following technical solutions:
The invention provides a preparation method of rare earth zirconate nano powder, which comprises the following steps:
mixing rare earth oxide, zirconia, molten salt and absolute ethyl alcohol to obtain a mixed material;
Calcining the mixed material to obtain the rare earth zirconate nano powder;
the molten salt comprises sodium chloride, potassium chloride and lithium chloride;
the mass ratio of the sodium chloride to the potassium chloride to the lithium chloride is 1: (1-5): (1-5);
The calcining temperature is 1000-1200 ℃, and the calcining time is 2-8 h.
Preferably, the rare earth oxide is one or two of lanthanum oxide, cedar oxide, gadolinium oxide, dysprosium oxide, neodymium oxide and ytterbium oxide.
preferably, the molar ratio of the rare earth oxide to the zirconia is 1: 2.
Preferably, the mass ratio of the total mass of the rare earth oxide and the zirconia to the molten salt is 1: (1-8).
Preferably, the mixing is performed under ball milling conditions;
The ball-material ratio of the ball mill is (1-3): 1, the rotating speed is 200-350 r/min, and the time is 10-24 h.
Preferably, the rare earth oxide is a nanoscale rare earth oxide, and the particle size of the nanoscale rare earth oxide is 20-50 nm;
The zirconia is nano-grade zirconia, and the particle size of the nano-grade zirconia is 20-50 nm.
The invention also provides the rare earth zirconate nano powder prepared by the preparation method in the technical scheme, wherein the particle size of the rare earth zirconate nano powder is 50-200 nm.
The invention also provides the application of the rare earth zirconate nano powder in the technical scheme in preparing refractory materials, thermal barrier coating materials, high-temperature solid electrolyte materials and main materials for fixing actinides in nuclear waste.
The invention provides a preparation method of rare earth zirconate nano powder, which comprises the following steps: mixing rare earth oxide, zirconia, molten salt and absolute ethyl alcohol to obtain a mixed material; calcining the mixed material to obtain the rare earth zirconate nano powder; the molten salt comprises sodium chloride, potassium chloride and lithium chloride; the mass ratio of the sodium chloride to the potassium chloride to the lithium chloride is 1: (1-5): (1-5); the calcining temperature is 1000-1200 ℃, and the calcining time is 2-8 h. The fused salt in the invention adopts the mixture of sodium chloride, potassium chloride and lithium chloride, so that the defects of corrosion of the traditional fused salt containing sulfate ions to production equipment and overhigh calcining temperature caused by high melting point can be avoided; meanwhile, the mass ratio of the sodium chloride to the potassium chloride to the lithium chloride is controlled within the range, so that the melting point of the molten salt can be reduced, and the low-temperature preparation of the lanthanum zirconate powder is realized. Meanwhile, the rare earth zirconate nano powder prepared by the preparation method has small particle size and uniform distribution. According to the description of the embodiment, the particle size of the rare earth zirconate nano-powder prepared by the preparation method is 50-200 nm.
drawings
FIG. 1 is a TEM image of lanthanum zirconate nanopowder prepared in example 1;
FIG. 2 is a TEM image of samarium zirconate nanopowder prepared in example 2;
FIG. 3 is a TEM image of samarium gadolinium zirconate nanopowder prepared in example 3.
Detailed Description
The invention provides a preparation method of rare earth zirconate nano powder, which comprises the following steps:
Mixing rare earth oxide, zirconia, molten salt and absolute ethyl alcohol to obtain a mixed material;
Calcining the mixed material to obtain the rare earth zirconate nano powder;
The molten salt comprises sodium chloride, potassium chloride and lithium chloride;
the mass ratio of the sodium chloride to the potassium chloride to the lithium chloride is 1: (1-5): (1-5);
The calcining temperature is 1000-1200 ℃, and the calcining time is 2-8 h.
in the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
Mixing rare earth oxide, zirconia, molten salt and absolute ethyl alcohol to obtain a mixed material; in the present invention, the rare earth oxide is preferably one or two of lanthanum oxide, cedar oxide, gadolinium oxide, dysprosium oxide, neodymium oxide and ytterbium oxide, and when the rare earth oxide is two of the above specific choices, the present invention does not have any special limitation on the proportion of the specific substances, and the specific substances may be mixed according to any proportion. In the invention, the rare earth oxide is preferably a nanoscale rare earth oxide, and the particle size of the nanoscale rare earth oxide is preferably 20-50 nm, and more preferably 25-40 nm. In the invention, the nano-scale rare earth oxide is selected to further reduce the preparation temperature of the rare earth zirconate powder, the particle size of the prepared powder reaches the nano level, and the sintering activity of the powder is improved.
In the invention, the zirconia is preferably nanoscale zirconia, and the particle size of the nanoscale zirconia is preferably 20-50 nm, and more preferably 25-40 nm. In the invention, the nano-grade zirconia is selected to further reduce the preparation temperature of the rare earth zirconate powder, the particle size of the prepared powder reaches the nano grade, and the sintering activity of the powder is improved.
in the present invention, the molar ratio of the rare earth oxide to zirconia is preferably 1: 2.
In the present invention, the mass ratio of sodium chloride, potassium chloride, and lithium chloride in the molten salt is preferably 1: (2-4): (2-4).
In the present invention, the mass ratio of the total mass of the rare earth oxide and zirconia to the molten salt is preferably 1: (1 to 8), more preferably 1: (2-7), most preferably 1: (3-5).
in the invention, the mass ratio of the zirconium oxide to the absolute ethyl alcohol is preferably 1 (10-20), more preferably 1: (12-18), most preferably 1: (15-17).
the order of mixing is not particularly limited in the present invention, and mixing may be performed by using a mixing order known to those skilled in the art.
in the present invention, the mixing is preferably performed under ball milling conditions; the ball-material ratio of the ball milling is preferably (1-3): 1, more preferably (1.5 to 2.5): 1, most preferably (1.8-2.2): the rotation speed of the ball milling is preferably 200-350 r/min, more preferably 250-300 r/min, most preferably 260-280 r/min, and the time of the ball milling is preferably 10-24 h, more preferably 12-20 h, and most preferably 15-18 h.
After the ball milling is finished, the ball-milled materials are preferably dried, and the drying temperature is preferably 80-120 ℃, more preferably 100 ℃; the drying time is preferably 20-30 h, more preferably 22-28 h, and most preferably 24-26 h. In the present invention, the drying is preferably drying.
After the mixed material is obtained, the mixed material is calcined to obtain the rare earth zirconate nano powder. In the invention, the calcining temperature is 1000-1200 ℃, preferably 1050-1150 ℃, and more preferably 1100-1150 ℃; the calcining time is 2-8 h, and more preferably 3-5 h; the rate of temperature rise to the temperature for the calcination is preferably 5 ℃/min. In the present invention, the calcination is preferably performed in a high-temperature furnace.
After the calcination is completed, the invention preferably sequentially cleans, filters and dries the calcined product. In the invention, the cleaning is preferably performed for 3 times by using deionized water; the suction filtration is not particularly limited in the present invention, and may be carried out by a process known to those skilled in the art. In the invention, the drying temperature is preferably 100 ℃, and the drying time is preferably 12 h; the drying mode is preferably drying.
The invention also provides the rare earth zirconate nano powder prepared by the preparation method in the technical scheme, wherein the particle size of the rare earth zirconate nano powder is 50-200 nm.
The invention also provides the application of the rare earth zirconate nano powder in the technical scheme in preparing refractory materials, thermal barrier coating materials, high-temperature solid electrolyte materials and main materials for fixing actinides in nuclear waste. The method of the present invention is not particularly limited, and those known to those skilled in the art can be used.
The rare earth zirconate nanopowder and the preparation method and application thereof provided by the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
Mixing 325.81g of nano lanthanum oxide, 246.44g of nano zirconium oxide, 343.35g of sodium chloride, 686.79g of potassium chloride, 702.82g of lithium chloride and 3433.5g of absolute ethyl alcohol, and carrying out ball milling for 12 hours, wherein the ball-material ratio is 2:1, the ball milling speed is 300 revolutions per minute, and drying for 12 hours at 100 ℃ to obtain a mixed material; placing the mixed material in a high-temperature furnace, heating to 1000 ℃ at a speed of 5 ℃/min, and preserving heat for 8 hours; washing with deionized water for 3 times, filtering, and drying at 100 ℃ for 12h to obtain lanthanum zirconate nano powder;
FIG. 1 is a TEM image of the lanthanum zirconate nanopowder, which shows that the average particle diameter of the lanthanum zirconate nanopowder is 50 nm.
example 2
Mixing 348.72g of nano samarium oxide, 246.44g of nano zirconium oxide, 330.64g of sodium chloride, 1322.56 g of potassium chloride, 1310.45g of lithium chloride and 3433.5g of absolute ethyl alcohol, carrying out ball milling for 12 hours, wherein the ball-material ratio is 2:1, the ball milling speed is 300 revolutions per minute, and drying for 24 hours at 100 ℃ to obtain a mixed material; placing the mixed material in a high-temperature furnace, heating to 1100 ℃ at a speed of 5 ℃/min, and preserving heat for 5 hours; washing with deionized water for 3 times, filtering, and drying at 100 ℃ for 24h to obtain lanthanum zirconate nano powder;
FIG. 2 is a TEM image of the lanthanum zirconate nanopowder, and it can be seen that the average particle diameter of the lanthanum zirconate nanopowder is 95 nm.
example 3
Mixing 174.36g of nano samarium oxide, 181.25g of nano gadolinium oxide, 344.03g of nano zirconium oxide, 1035.62g of potassium chloride, 1032.09g of lithium chloride and 3433.5g of absolute ethyl alcohol, and carrying out ball milling for 12 hours at a ball-material ratio of 2:1 at a ball-milling rotation speed of 300 revolutions per minute and drying at 100 ℃ for 26 hours to obtain a mixed material; placing the mixed material in a high-temperature furnace, heating to 1200 ℃ at a speed of 5 ℃/min, and preserving heat for 3 h; washing with deionized water for 3 times, performing suction filtration and drying at 100 ℃ for 24 hours to obtain samarium gadolinium zirconate nano-powder;
FIG. 3 is a TEM image of the samarium-gadolinium zirconate nano-powder, and it can be seen from the image that the average particle size of the samarium-gadolinium zirconate nano-powder is 200 nm.
Example 4
162.91g of nano lanthanum oxide, 186.5g of nano dysprosium oxide, 246.44g of nano zirconium oxide, 260.68g of sodium chloride, 912.39g of potassium chloride and 4000g of absolute ethyl alcohol in 918.85g of lithium chloride are mixed and ball-milled for 12 hours, the ball-milling speed is 300 r/min, and the mixture is dried for 24 hours at 100 ℃ to obtain a mixed material, wherein the ball-milling speed is 2: 1; placing the mixed material in a high-temperature furnace, heating to 1150 ℃ at a speed of 5 ℃/min, and preserving heat for 8 hours; washing the lanthanum dysprosium zirconate nano powder for 3 times by using deionized water, carrying out suction filtration and drying for 24 hours at 100 ℃ to obtain the lanthanum dysprosium zirconate nano powder, wherein the average particle size of the lanthanum dysprosium zirconate nano powder is 180 nm.
Example 5
168.24g of nano neodymium oxide, 197.04g of nano ytterbium oxide, 246.44g of nano zirconium oxide, 275.27g of sodium chloride, 1238.73 g of potassium chloride, 1256.82g of lithium chloride and 4000g of absolute ethyl alcohol are mixed and ball-milled for 12 hours, the ball-material ratio is 2:1, the ball-milling rotating speed is 300 r/min, and the mixture is dried for 26 hours at the temperature of 100 ℃ to obtain a mixed material; placing the mixed material in a high-temperature furnace, heating to 1100 ℃ at a speed of 5 ℃/min, and preserving heat for 8 hours; and washing the neodymium zirconate ytterbium nano powder for 3 times by using deionized water, performing suction filtration and drying the neodymium zirconate ytterbium nano powder for 24 hours at 100 ℃ to obtain the neodymium zirconate ytterbium nano powder, wherein the average particle size of the neodymium zirconate ytterbium nano powder is 140 nm.
The embodiments show that the preparation method provided by the invention is simple, the synthesis temperature is low, the cost is low, and the prepared rare earth zirconate powder is nano-scale.
the foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The preparation method of the rare earth zirconate nano powder is characterized by comprising the following steps of:
mixing rare earth oxide, zirconia, molten salt and absolute ethyl alcohol to obtain a mixed material;
Calcining the mixed material to obtain the rare earth zirconate nano powder;
the molten salt comprises sodium chloride, potassium chloride and lithium chloride;
The mass ratio of the sodium chloride to the potassium chloride to the lithium chloride is 1: (1-5): (1-5);
The calcining temperature is 1000-1200 ℃, and the calcining time is 2-8 h.
2. The method according to claim 1, wherein the rare earth oxide is one or two of lanthanum oxide, cedar oxide, gadolinium oxide, dysprosium oxide, neodymium oxide, and ytterbium oxide.
3. The production method according to claim 1 or 2, wherein the molar ratio of the rare earth oxide to the zirconia is 1: 2.
4. the production method according to claim 3, wherein the mass ratio of the total mass of the rare earth oxide and zirconia to the molten salt is 1: (1-8).
5. The method of claim 1, wherein the mixing is performed under ball milling conditions;
The ball-material ratio of the ball mill is (1-3): 1, the rotating speed is 200-350 r/min, and the time is 10-24 h.
6. The method according to claim 1 or 2, wherein the rare earth oxide is a nano-sized rare earth oxide having a particle size of 20 to 50 nm;
The zirconia is nano-grade zirconia, and the particle size of the nano-grade zirconia is 20-50 nm.
7. The rare earth zirconate nanopowder prepared by the preparation method of any one of claims 1 to 6, wherein the particle size of the rare earth zirconate nanopowder is 50 to 200 nm.
8. The use of the rare earth zirconate nanopowder of claim 7 in the host materials for the fixation of actinides in refractory materials, thermal barrier coating materials, high temperature solid electrolyte materials and nuclear waste.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111153434A (en) * | 2020-01-17 | 2020-05-15 | 华南理工大学 | Preparation method of lanthanum zirconate spherical powder for thermal spraying |
| CN112340777A (en) * | 2020-10-30 | 2021-02-09 | 中科立民新材料（扬州）有限公司 | Method for synthesizing pure lanthanum chromate at low temperature, lanthanum chromate synthesized by method and application of lanthanum chromate |
| CN113430330A (en) * | 2021-06-23 | 2021-09-24 | 北京浩德楚业新材料科技有限公司 | Preparation method of zirconia solid electrolyte tube and oxygen determination probe |
| CN115010171A (en) * | 2022-05-19 | 2022-09-06 | 北京科技大学 | Green preparation method of nano lanthanum zirconate powder |
| CN115536062A (en) * | 2022-11-02 | 2022-12-30 | 中国科学院过程工程研究所 | Solid-phase synthesis method of lanthanum zirconate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111153434A (en) * | 2020-01-17 | 2020-05-15 | 华南理工大学 | Preparation method of lanthanum zirconate spherical powder for thermal spraying |
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| CN113430330A (en) * | 2021-06-23 | 2021-09-24 | 北京浩德楚业新材料科技有限公司 | Preparation method of zirconia solid electrolyte tube and oxygen determination probe |
| CN115010171A (en) * | 2022-05-19 | 2022-09-06 | 北京科技大学 | Green preparation method of nano lanthanum zirconate powder |
| CN115536062A (en) * | 2022-11-02 | 2022-12-30 | 中国科学院过程工程研究所 | Solid-phase synthesis method of lanthanum zirconate |
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Application publication date: 20191213 |
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