CN106348342B - A kind of preparation method of spherical zirconic acid lanthanum nano material - Google Patents
A kind of preparation method of spherical zirconic acid lanthanum nano material Download PDFInfo
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- CN106348342B CN106348342B CN201610816334.5A CN201610816334A CN106348342B CN 106348342 B CN106348342 B CN 106348342B CN 201610816334 A CN201610816334 A CN 201610816334A CN 106348342 B CN106348342 B CN 106348342B
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/30—Particle morphology extending in three dimensions
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Abstract
The invention belongs to inorganic non-metallic material preparation field, a kind of more particularly to spherical zirconic acid lanthanum preparation method of nano material, after it is so that lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium fully to be dissolved in methanol solution, carry out solvent thermal reaction, after filtering, washing, spherical zirconic acid lanthanum nano material is produced after drying, calcining cooling.Present invention process is simple and easy to do, product purity is high, preparation cost is low, and the size of products obtained therefrom is 150 ~ 200 nm, and the homogeneity of product, dispersiveness are all fine, and simple production process, and sintering temperature is low, is readily applied to actual large-scale production.Spherical zirconic acid lanthanum nano material being with a wide range of applications in high temperature insulating field prepared by the present invention.
Description
Technical field
The invention belongs to the preparing technical field of inorganic non-metallic material, concretely relates to a kind of spherical zirconic acid lanthanum and receives
The preparation method of rice material.
Background technology
Zirconic acid lanthanum（La2Zr2O7）For A2B2O7Type binary metal oxide material, crystal structure is identical with pyrochlore, and category is vertical
Prismatic crystal system, it can also regard what is be derived by fluorite structure as.Because its excellent crystal structure determines that zirconic acid lanthanum has very
More special property, the especially application in high temperature thermal insulation coating field are very extensive.The combustion gas wheel that aerospace field uses
Machine develops to high inlet temperature, high thrust-weight ratio direction, and the pressure of the fuel gas temperature in combustion chamber improves very much, it is desirable to manufactures combustion gas wheel
Material used in machine must possess the performances such as high-melting-point, high thermal expansion coefficient, good inoxidizability and corrosion resistance.Pyrochlore
The zirconic acid lanthanum material of type structure has excellent high temperature phase stability, and crystal structure is kept not before fusing point (2300 °C)
Become.Compared with traditional zirconium oxide, zirconic acid lanthanum in room temperature to, without phase in version, heat endurance is higher between fusing point, thermal conductivity factor, heat
The coefficient of expansion and Young's modulus are lower, more anti-sintering.Due to the above-described outstanding advantages of zirconic acid lanthanum material, zirconic acid lanthanum nanometer material
Expect being with a wide range of applications in high temperature insulating field.
The preparation method of zirconic acid lanthanum nano material includes solid reaction process, self-propagating combustion, chemical coprecipitation, molten
Glue-gel method, sol-gel auto-combustion, hydro-thermal method etc..Solid-phase sintering reaction method is to prepare the most frequently used method of powder
One of, but the composition in product easily produces deviation, and more than 1450 °C of single-phase calcining heat.Sol-gel process method
Though the method that more satisfactory easy-to-use prepares high-active superfine powder end, will typically use expensive alkoxide,
It is unfavorable to application.Self-propagating combustion step is simple, does not need complex device, can prepare at a lower temperature single
The ultra-fine zirconic acid lanthanum powder of phase composition, but in combustion, material experienced very big temperature change, very high heating and
Cooldown rate increases in product defect to have impact on its performance.
The content of the invention
It is contemplated that provide a kind of technique in place of overcome the deficiencies in the prior art simple, purpose product high income, system
Standby cost is low, the preparation method of the high spherical zirconic acid lanthanum nano material of product purity.
To reach above-mentioned purpose, what the present invention was realized in.
A kind of preparation method of spherical zirconic acid lanthanum nano material, is to fill lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium in methyl alcohol
After dividing dissolving, solvent thermal reaction is carried out, after filtering, washing, drying, produces purpose product after calcining cooling.
As a kind of preferred scheme, the mol ratio of lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium of the present invention is 1:1.The second
The molar concentration of acyl acetone lanthanum is 0.01~0.1 mol/L.
Further, for solvent thermal reaction temperature of the present invention at 110~220 °C, the reaction time is 6~48 hours.
Further, drying time of the present invention is 1~5 hour, and drying temperature is 60~150 °C, heating rate
For 2~10 °C/minute.
Further, calcination time of the present invention is 2~8 hours, and calcining heat is 600~800 °C, heating speed
Rate is 2~20 °C/minute.
The present invention utilizes solvent heat-calcining two-step method, has successfully prepared higher spherical of purity under cryogenic
Zirconic acid lanthanum nano material.
Compared with prior art, the present invention has following features.
（1）The preparation technology route of spherical zirconic acid lanthanum nano material is simple, and preparation cost is low, easy to control.Not
Can prepares the zirconic acid lanthanum nano material of pure phase under conditions of higher than 800 °C, and production efficiency is higher, and purpose product is received
Rate is 99.0%~99.9%.
（2）The spherical zirconic acid lanthanum nano material of purpose product, its purity are high（99.92%~99.98%）, impurity content is low,
Good dispersion（It can be seen that by SEM figures）.
（3）It is spherical morphology to synthesize zirconic acid lanthanum material, and the size of ball is 150 ~ 200 nm, can meet industrial application pair
The requirement of spherical zirconic acid lanthanum nano material product.
Brief description of the drawings
The invention will be further described with reference to the accompanying drawings and detailed description.Protection scope of the present invention not only office
It is limited to the statement of following content.
Fig. 1 is the SEM shape appearance figures of the spherical zirconic acid lanthanum nano material prepared by the present invention.
Fig. 2 is the SEM shape appearance figures of the spherical zirconic acid lanthanum nano material prepared by the present invention.
Fig. 3 is the SEM shape appearance figures of the spherical zirconic acid lanthanum nano material prepared by the present invention.
Fig. 4 is the SEM shape appearance figures of the spherical zirconic acid lanthanum nano material prepared by the present invention.
Fig. 5 is the SEM shape appearance figures of the spherical zirconic acid lanthanum nano material prepared by the present invention.
Fig. 6 is the X-ray diffraction pattern figure of the spherical zirconic acid lanthanum nano material prepared by the present invention.
Embodiment
After the present invention fully dissolves lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium in methyl alcohol, solvent thermal reaction is carried out（Temperature
At 110~220 °C, the time is 6~48 hours）, filtering, washing, dry, produce purpose product after calcining cooling（Drying time
For 1~5 hour, temperature was 60~120 °C, and heating rate is 2~10 °C/minute.Calcination time is 2~8 hours, and temperature is
600~800 °C, heating rate is 2~20 °C/minute）.
Its preparation process is.
（1）By lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium according to certain molar ratio weighing after, be put into methanol and fully dissolve.
By obtained mixed solution at a certain temperature, solvent thermal reaction is carried out, solvent thermal reaction temperature is at 110~220 °C, solvent
The thermal response time is 6~48 hours.
（2）Solvent thermal reaction terminates, and after naturally cooling to room temperature, baking is put into after reacting obtained product filtering, washing
In case, programmed rate is 2~10 °C/minute, under the conditions of 60~120 °C, is dried 1~5 hour.
（3）It is above-mentioned it is dried after, resulting product is directly calcined in Muffle furnace, Muffle furnace Program heating liter
Warm speed range is in 2~20 °C/min.Calcination time is 2~8 hours, and calcining heat is 600~800 °C.After natural cooling i.e.
Spherical zirconic acid lanthanum nano material is made.
Referring to the ESEM shown in Fig. 1~5, carried out for the spherical zirconic acid lanthanum nano material prepared by the present invention（SEM）
Figure, the spherical zirconic acid lanthanum nano material of products obtained therefrom, the size of nano-particle is 150~200 nm.Fig. 6 is prepared by the present invention
The X-ray diffraction pattern figure of spherical zirconic acid lanthanum nano material, its PDF card number are：17-0450.
Embodiment 1.
According to mol ratio it is 1 by lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium：1, methanol is put into after precise（12C,
99.95%）Middle stirring and dissolving, the molar concentration of lanthanum acetylacetone is 0.01 mol/L.Obtained mixed solution is subjected to solvent heat
Reaction, for solvent thermal reaction temperature at 200 °C, the solvent thermal reaction time is 24 hours.After solvent thermal reaction terminates, natural cooling
To room temperature, it is put into after the product filtration washing that reaction is obtained in baking oven, °C/minute of programmed rate 5, in 120 °C of bars
Dried 5 hours under part.Then it is placed in Muffle furnace and calcines, calcination time is 8 hours, and calcining heat is 600 °C, heating rate
For 10 °C/minute.Spherical zirconic acid lanthanum nano material is obtained after natural cooling, and the size of ball is 160 nm, the yield of its product
For 99.9%.Product purity is 99.98%, and impurity carbon content is less than 0.02%.
Embodiment 2.
According to mol ratio it is 1 by lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium：1, methanol is put into after precise（12C,
99.95%）Middle stirring and dissolving, the molar concentration of lanthanum acetylacetone is 0.05 mol/L.Obtained mixed solution is subjected to solvent heat
Reaction, for solvent thermal reaction temperature at 220 °C, the solvent thermal reaction time is 12 hours.After solvent thermal reaction terminates, natural cooling
To room temperature, it is put into after the product filtration washing that reaction is obtained in baking oven, °C/minute of programmed rate 5, in 120 °C of bars
Dried 5 hours under part.Then it is placed in Muffle furnace and calcines, calcination time is 2 hours, and calcining heat is 800 °C, heating rate
For 20 °C/minute.Spherical zirconic acid lanthanum nano material is obtained after natural cooling, and the size of ball is 150 nm, the yield of its product
For 99.0%.Product purity is 99.96%, and impurity carbon content is less than 0.04%.
Embodiment 3.
According to mol ratio it is 1 by lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium：1, methanol is put into after precise（12C,
99.95%）Middle stirring and dissolving, the molar concentration of lanthanum acetylacetone is 0.1 mol/L.Obtained mixed solution is subjected to solvent heat
Reaction, for solvent thermal reaction temperature at 200 °C, the solvent thermal reaction time is 48 hours.After solvent thermal reaction terminates, natural cooling
To room temperature, it is put into after the product filtration washing that reaction is obtained in baking oven, °C/minute of programmed rate 5, in 120 °C of bars
Dried 5 hours under part.Then it is placed in Muffle furnace and calcines, calcination time is 8 hours, and calcining heat is 800 °C, heating rate
For 10 °C/minute.Spherical zirconic acid lanthanum nano material is obtained after natural cooling, and the size of ball is 200 nm, the yield of its product
For 99.7%.Product purity is 99.97%, and impurity carbon content is less than 0.03%.
Embodiment 4.
According to mol ratio it is 1 by lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium：1, methanol is put into after precise（12C,
99.95%）Middle stirring and dissolving, the molar concentration of lanthanum acetylacetone is 0.02 mol/L.Obtained mixed solution is subjected to solvent heat
Reaction, for solvent thermal reaction temperature at 110 °C, the solvent thermal reaction time is 48 hours.After solvent thermal reaction terminates, natural cooling
To room temperature, it is put into after the product filtration washing that reaction is obtained in baking oven, °C/minute of programmed rate 10, in 120 °C of bars
Dried 5 hours under part.Then it is placed in Muffle furnace and calcines, calcination time is 8 hours, and calcining heat is 700 °C, heating rate
For 20 °C/minute.Spherical zirconic acid lanthanum nano material is obtained after natural cooling, and the size of ball is 200 nm, the yield of its product
For 99.8%.Product purity is 99.92%, and impurity carbon content is less than 0.08%.
Embodiment 5.
According to mol ratio it is 1 by lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium：1, methanol is put into after precise（12C,
99.95%）Middle stirring and dissolving, the molar concentration of lanthanum acetylacetone is 0.04 mol/L.Obtained mixed solution is subjected to solvent heat
Reaction, for solvent thermal reaction temperature at 220 °C, the solvent thermal reaction time is 12 hours.After solvent thermal reaction terminates, natural cooling
To room temperature, it is put into after the product filtration washing that reaction is obtained in baking oven, °C/minute of programmed rate 5, in 120 °C of bars
Dried 5 hours under part.Then it is placed in Muffle furnace and calcines, calcination time is 8 hours, and calcining heat is 600 °C, heating rate
For 20 °C/minute.Spherical zirconic acid lanthanum nano material is obtained after natural cooling, and the size of ball is 180 nm, the yield of its product
For 99.2%.Product purity is 99.95%, and impurity carbon content is less than 0.05%.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (5)
- A kind of 1. preparation method of spherical zirconic acid lanthanum nano material, it is characterised in that:Lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium are pressed It is 1 according to mol ratio：1, stirring and dissolving in methanol is put into after precise, and the molar concentration of lanthanum acetylacetone is 0.01mol/L；Will Obtained mixed solution carries out solvent thermal reaction, and for solvent thermal reaction temperature at 200 DEG C, the solvent thermal reaction time is 24 hours；It is molten After agent thermal response terminates, room temperature is naturally cooled to, is put into after the product filtration washing that reaction is obtained in baking oven, temperature programming speed 5 DEG C/min of rate, dried 5 hours under the conditions of 120 DEG C；Then it is placed in Muffle furnace and calcines, calcination time is 8 hours, calcining Temperature is 600 DEG C, and heating rate is 10 DEG C/min；Spherical zirconic acid lanthanum nano material is obtained after natural cooling, the size of ball is 160nm, the yield of its product is 99.9%；Product purity is 99.98%, and impurity carbon content is less than 0.02%.
- A kind of 2. preparation method of spherical zirconic acid lanthanum nano material, it is characterised in that:Lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium are pressed It is 1 according to mol ratio：1, stirring and dissolving in methanol is put into after precise, and the molar concentration of lanthanum acetylacetone is 0.05mol/L；Will Obtained mixed solution carries out solvent thermal reaction, and for solvent thermal reaction temperature at 220 DEG C, the solvent thermal reaction time is 12 hours；It is molten After agent thermal response terminates, room temperature is naturally cooled to, is put into after the product filtration washing that reaction is obtained in baking oven, temperature programming 5 DEG C/min of speed, dried 5 hours under the conditions of 120 DEG C；Then it is placed in Muffle furnace and calcines, calcination time is 2 hours, is forged It is 800 DEG C to burn temperature, and heating rate is 20 DEG C/min；Spherical zirconic acid lanthanum nano material, the size of ball are obtained after natural cooling For 150 nm, the yield of its product is 99.0%；Product purity is 99.96%, and impurity carbon content is less than 0.04%.
- A kind of 3. preparation method of spherical zirconic acid lanthanum nano material, it is characterised in that:Lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium are pressed It is 1 according to mol ratio：1, stirring and dissolving in methanol is put into after precise, and the molar concentration of lanthanum acetylacetone is 0.1mol/L；Will Obtained mixed solution carries out solvent thermal reaction, and for solvent thermal reaction temperature at 200 DEG C, the solvent thermal reaction time is 48 hours；It is molten After agent thermal response terminates, room temperature is naturally cooled to, is put into after the product filtration washing that reaction is obtained in baking oven, temperature programming speed 5 DEG C/min of rate, dried 5 hours under the conditions of 120 DEG C；Then it is placed in Muffle furnace and calcines, calcination time is 8 hours, calcining Temperature is 800 DEG C, and heating rate is 10 DEG C/min；Spherical zirconic acid lanthanum nano material is obtained after natural cooling, the size of ball is 200nm, the yield of its product is 99.7%；Product purity is 99.97%, and impurity carbon content is less than 0.03%.
- A kind of 4. preparation method of spherical zirconic acid lanthanum nano material, it is characterised in that:Lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium are pressed It is 1 according to mol ratio：1, stirring and dissolving in methanol is put into after precise, and the molar concentration of lanthanum acetylacetone is 0.02 mol/L； Obtained mixed solution is subjected to solvent thermal reaction, for solvent thermal reaction temperature at 110 DEG C, the solvent thermal reaction time is 48 hours； After solvent thermal reaction terminates, room temperature is naturally cooled to, is put into after the product filtration washing that reaction is obtained in baking oven, temperature programming 10 DEG C/min of speed, dried 5 hours under the conditions of 120 DEG C, be then placed in Muffle furnace and calcine, calcination time is 8 hours, is forged It is 700 DEG C to burn temperature, and heating rate is 20 DEG C/min；Spherical zirconic acid lanthanum nano material, the size of ball are obtained after natural cooling For 200nm, the yield of its product is 99.8%；Product purity is 99.92%, and impurity carbon content is less than 0.08%.
- A kind of 5. preparation method of spherical zirconic acid lanthanum nano material, it is characterised in that:Lanthanum acetylacetone and acetylacetone,2,4-pentanedione zirconium are pressed It is 1 according to mol ratio：1, stirring and dissolving in methanol is put into after precise, and the molar concentration of lanthanum acetylacetone is 0.04mol/L；Will Obtained mixed solution carries out solvent thermal reaction, and for solvent thermal reaction temperature at 220 DEG C, the solvent thermal reaction time is 12 hours；It is molten After agent thermal response terminates, room temperature is naturally cooled to, is put into after the product filtration washing that reaction is obtained in baking oven, temperature programming speed 5 DEG C/min of rate, dried 5 hours under the conditions of 120 DEG C；Then it is placed in Muffle furnace and calcines, calcination time is 8 hours, calcining Temperature is 600 DEG C, and heating rate is 20 DEG C/min；Spherical zirconic acid lanthanum nano material is obtained after natural cooling, the size of ball is 180nm, the yield of its product is 99.2%；Product purity is 99.95%, and impurity carbon content is less than 0.05%.
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| CN101407336A (en) * | 2008-06-30 | 2009-04-15 | 中国科学院上海硅酸盐研究所 | Method for preparing lanthanum zirconate powder |
| CN103896620A (en) * | 2014-03-11 | 2014-07-02 | 中国人民解放军国防科学技术大学 | Hierarchic porous La2Zr2O7 ceramic and preparation method thereof |
| CN105905940A (en) * | 2016-04-12 | 2016-08-31 | 渤海大学 | Preparation method of nickel titanate/titanium dioxide composite nanomaterial |
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Patent Citations (3)
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| CN101407336A (en) * | 2008-06-30 | 2009-04-15 | 中国科学院上海硅酸盐研究所 | Method for preparing lanthanum zirconate powder |
| CN103896620A (en) * | 2014-03-11 | 2014-07-02 | 中国人民解放军国防科学技术大学 | Hierarchic porous La2Zr2O7 ceramic and preparation method thereof |
| CN105905940A (en) * | 2016-04-12 | 2016-08-31 | 渤海大学 | Preparation method of nickel titanate/titanium dioxide composite nanomaterial |
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