CN104355617A - High-temperature and high-pressure preparation method of cubic phase lanthanum, iron and titanium oxide - Google Patents
High-temperature and high-pressure preparation method of cubic phase lanthanum, iron and titanium oxide Download PDFInfo
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Abstract
The invention discloses a high-temperature and high-pressure preparation method of cubic phase lanthanum, iron and titanium oxide, and belongs to the technical field of the preparation of novel functional ceramic material. The method comprises steps that La(NO3)3, Fe(NO3)3 and C16H36O4Ti are taken as raw material and prepared into precursor through a sol-gel method, and the precursor is subjected to processes of briquetting, assembly, high-temperature and high-pressure synthesis and cooling depressurization, so as to obtain the cubic phase material with the constituent being La2TeTiO6. The product prepared is small in grain size and high in purity; high-temperature and high-pressure equipment adopted is simple to operate and can rapidly carry out industrialization, and high-quality lanthanum, iron and titanium oxide cubic phase material can be obtained.
Description
Technical field
The invention belongs to technical field prepared by new function stupalith.Be specifically related to the Emission in Cubic of lanthanum iron titanium oxide, and with lanthanum nitrate (La (NO
3)
3), iron nitrate (Fe (NO
3)
3), butyl (tetra) titanate (C
16h
36o
4ti) be raw material, utilize the method for High Temperature High Pressure technology of preparing synthesis of cubic phase lanthanum iron titanium oxide.
Background technology
The preparation of new calcium titanium ore, double-perovskite oxide high-temperature high-pressure process and research, for the research and apply of new function stupalith lays the foundation.The general formula of two calcium nutrition oxide compound can be expressed as A
2b ' B " O
6, " Sauerstoffatom of atom and its nearest neighbour forms B ' O for B ', B
6, B " O
6octahedron, these two kinds of octahedrons form three-dimensional network regularly alternately, and A atom is positioned among 8 adjacent octahedral spaces.Due to B ' and B, " ion has different electronic configurations, different ionic radius and exchange interaction dissimilar each other, thus to the replacement of B position ion, the powerful measure of the physical essence becoming its inherence of further investigation of adulterating.From application point, novel pair of calcium nutrition rare earth oxide can provide more abundant functional property, has very large potentiality to be exploited in the field such as environment protection and Industrial Catalysis.Lanthanum iron titanium oxide (the La (comprising solid phase method, sol-gel method etc.) under current normal condition and prepare
2feTiO
6) crystalline structure of material is tetragonal.Also do not report at present about the preparation of employing High Temperature High Pressure.The kind adding this type oxide is can be described as mutually by the new texture of research lanthanum iron titanium oxide, and the different new chemical catalysis function thereupon produced, and the application of Industrial Catalysis aspect can be increased in.
Summary of the invention
The technical problem to be solved in the present invention adopts the new method preparing lanthanum iron titanium oxide material-HP-HT synthesize method, the method adjusts the formation of the high pressure phase structure of lanthanum iron titanium oxide mainly through synthesis temperature and pressure, prepare the high pressure phase material of the lanthanum iron titanium oxide with brand-new structure; And the method is easy to implement.
Lanthanum iron titanium oxide new texture phase of the present invention, component is La
2feTiO
6, its structure is cubic structure.
Concrete technical scheme prepared by Emission in Cubic lanthanum iron titanium oxide of the present invention is as described below.
A preparation method for lanthanum iron titanium oxide Emission in Cubic, with lanthanum nitrate (La (NO
3)
3), iron nitrate (Fe (NO
3)
3), butyl (tetra) titanate (C
16h
36o
4ti) be raw material, obtain precursor by sol-gel method, precursor is obtained lanthanum iron titanium oxide Emission in Cubic material through the technological process of briquetting, assembling, HP-HT synthesize, cooling release; Described precursor, is by 2: 1: 1 mixing in molar ratio of lanthanum nitrate, iron nitrate, butyl (tetra) titanate, prepares gained by sol-gel method; Described briquetting is the precursor that will obtain, and is pressed into sheet by boron nitride (BN) pipe diameter; Said assembling, is sheet-shaped material is loaded boron nitride (BN) pipe, and boron nitride tube is loaded carbon tube heating container, then put into pyrophyllite synthetic cavity; Said HP-HT synthesize carries out on the cubic pressure machine equipment required for high temperature and high pressure method, pressure be 5GPa, temperature be 850 ~ 1050 DEG C at heat-insulation pressure keeping 15 ~ 30 minutes; Described cooling release naturally cools to release after room temperature after stopping heating.
Described cooling release, can also be stop the rear first pressurize release after 5 ~ 10 minutes of heating, then naturally cool to room temperature.Be conducive to like this reducing dephasign, be conducive to the protection of equipment and reduce the duration of service of press, improve the service efficiency of press.
Above-mentioned technical scheme also can be stated as:
A high temperature and high pressure preparation process for Emission in Cubic lanthanum iron titanium oxide, the processing step through obtained precursor and HP-HT synthesize obtains Emission in Cubic lanthanum iron titanium oxide;
Described obtained precursor, be with lanthanum nitrate, iron nitrate, butyl (tetra) titanate in molar ratio 2: 1: 1 for raw material, obtained by sol-gel method;
Described HP-HT synthesize, high temperature high pressure device is carried out; Precursor is ground to form powdery compression moulding again, outside parcel boron nitride (BN) layer, loads in pyrophyllite synthetic cavity; Pressure be 5GPa, at temperature is 850 ~ 1050 DEG C, heat-insulation pressure keeping 15 ~ 30 minutes, cooling release.
Above-mentioned obtained precursor, can obtain by the sol-gel method of prior art, also can obtain according to the following procedure: butyl (tetra) titanate is joined in mass concentration 95% ethanol, produce white precipitate, drip concentrated nitric acid wherein to dissolve completely to precipitation, obtain butyl (tetra) titanate clear solution; By La (NO
3)
3with Fe (NO
3)
3be dissolved in deionized water, then add glucose or the citric acid of butyl (tetra) titanate clear solution and 4.6 ~ 4.9 times of butyl (tetra) titanate mole numbers, stir and be warming up to 70 DEG C, constant temperature is stirred to solution and becomes thickness formation colloidal sol, and rebake obtains dry bulk colloid; 3 hours are sintered, obtained precursor by 500 DEG C, colloid.
Described baking, can at 110 DEG C dry 24 hours.
Described lanthanum nitrate (La (NO
3)
3), iron nitrate (Fe (NO
3)
3), butyl (tetra) titanate (C
16h
36o
4ti) be raw material, their quality purity>=99.9%.
Compound experiment of the present invention can complete on domestic DS029B type six-plane piercer.The temperature height of synthesis, heat-insulation pressure keeping time are the important factors affecting Emission in Cubic lanthanum iron titanium oxide purity, and the present invention is best, and synthesis pressure is 5GPa, and optimum synthesising temperature is 950 DEG C, and the time of heat-insulation pressure keeping is 15 minutes.
The present invention also asks to protect the product adopting the high temperature and high pressure preparation process of Emission in Cubic lanthanum iron titanium oxide of the present invention to obtain.The component of product is La
2feTiO
6, its structure is cubic structure.
Beneficial effect of the present invention is, the first, and present method first utilizes sol-gel method to prepare precursor, and reactant is mixed, and products therefrom particle diameter is little, and the final product Emission in Cubic lanthanum iron titanium oxide purity of gained is high.Second, the high-temperature high-pressure apparatus that the lanthanum iron titanium oxide that present method is produced adopts is used for producing diamond at present at home in a large number, it is simple to operate, can implement industrialization quickly with its production, and can obtain the lanthanum iron titanium oxide Emission in Cubic material of high-quality.
Accompanying drawing explanation
Fig. 1 is lanthanum iron titanium oxide (La prepared by embodiment 1 High Temperature High Pressure
2feTiO
6) X-ray diffractogram.
Fig. 2 is lanthanum iron titanium oxide (La prepared by embodiment 2 High Temperature High Pressure
2feTiO
6) X-ray diffractogram.
Fig. 3 is lanthanum iron titanium oxide (La prepared by embodiment 3 High Temperature High Pressure
2feTiO
6) X-ray diffractogram.
Fig. 4 is lanthanum iron titanium oxide (La prepared by embodiment 4 High Temperature High Pressure
2feTiO
6) X-ray diffractogram.
Fig. 5 is lanthanum iron titanium oxide (La prepared by comparative example 1 sol-gel method
2feTiO
6) X-ray diffractogram.
Embodiment
Embodiment 1:
By butyl (tetra) titanate (C
16h
36o
4ti) join in a small amount of 95% ethanol, produce white precipitate, drip appropriate concentrated nitric acid wherein, until precipitation is dissolved completely, obtain butyl (tetra) titanate clear solution; La (NO in molar ratio
3)
3, Fe (NO
3)
3and C
16h
36o
4ti takes La (NO at 2: 1: 1
3)
3with Fe (NO
3)
3and be dissolved in deionized water, add glucose again, the consumption of glucose is 4.8 times of butyl (tetra) titanate by molar basis, then adds wherein by the butyl (tetra) titanate clear solution obtained above, makes its abundant complexing, 70 DEG C of constant temperature water baths stir and form gel, at 110 DEG C, drying must do glue in 24 hours, and dry glue, through 500 DEG C of roastings 3 hours, obtains precursor.By precursor abrasive dust, the flap-type precursor being then pressed into suitably height loads BN pipe, then is loaded in pyrophyllite synthetic cavity by sample.Make heating tube with graphite in synthetic cavity, do insulation tube with agalmatolite.Sample synthesis pressure be 5GPa, at temperature is 950 DEG C, 15 minutes pressure-maintaining and heat-preservation time, after stopping heating, sample naturally cools to release after room temperature.Emission in Cubic lanthanum iron titanium oxide (La prepared by this condition
2feTiO
6) crystallization degree is best, purity is the highest, and concrete X-ray diffraction spectra the results are shown in Figure 1.
Glucose in the present embodiment can substitute with the citric acid of identical mole number, and effect is the same.
Embodiment 2:
Adopt the identical precursor of embodiment 1 and assembling, synthesis pressure is 5GPa, and temperature is 950 DEG C, 30 minutes pressure-maintaining and heat-preservation time, and after stopping heating, sample naturally cools to release after room temperature.Cubic structure La prepared by this condition
2feTiO
6there is dephasign, concrete X-ray diffraction spectra the results are shown in Figure 2.
Embodiment 3:
Adopt the precursor identical with embodiment 1 and assembling, synthesis pressure is 5GPa, and temperature is 850 DEG C, 15 minutes pressure-maintaining and heat-preservation time, stop heating afterwards sample naturally cool to release after room temperature, cubic structure La prepared by this condition
2feTiO
6there is dephasign.Concrete X-ray diffraction spectra the results are shown in Figure 3.
Embodiment 4:
Adopt the precursor identical with embodiment 1 and assembling, synthesis pressure is 5GPa, and temperature is 1050 DEG C, 15 minutes pressure-maintaining and heat-preservation time, stop heating afterwards sample naturally cool to release after room temperature, cubic structure La prepared by this condition
2feTiO
6containing more dephasign.Concrete X-ray diffraction spectra the results are shown in Figure 4.
Comparative example 1
A certain amount of butyl (tetra) titanate is joined in a small amount of 95% ethanol, produce white precipitate, drip appropriate concentrated nitric acid wherein, until precipitation is dissolved completely, obtain clear solution.Lanthanum nitrate, iron nitrate and butyl (tetra) titanate are take lanthanum nitrate (La (NO at 2: 1: 1 in molar ratio
3)
36H
2and iron nitrate (Fe (NO O)
3)
39H
2o), and be dissolved in deionized water, add the glucose that molar basis is 4.8 times of butyl (tetra) titanate again, then add wherein by the clear solution obtained above, make its abundant complexing, 70 DEG C of constant temperature water baths stir and form gel, at 110 DEG C, drying must do glue in 24 hours, dry glue was through 500 DEG C of presintering 3 hours, and the sample that presintering obtains is again through grinding, compressing tablet, and then at 850 DEG C of temperature, sintering obtains Tetragonal La in 12 hours
2feTiO
6.Concrete X-ray the results are shown in Figure 5.
Claims (6)
1. a high temperature and high pressure preparation process for Emission in Cubic lanthanum iron titanium oxide, the processing step through obtained precursor and HP-HT synthesize obtains Emission in Cubic lanthanum iron titanium oxide;
Described obtained precursor, be with lanthanum nitrate, iron nitrate, butyl (tetra) titanate in molar ratio 2: 1: 1 for raw material, obtained by sol-gel method;
Described HP-HT synthesize, high temperature high pressure device is carried out; Precursor is ground to form powdery compression moulding again, outside parcel boron nitride layer, loads in pyrophyllite synthetic cavity; Pressure be 5GPa, at temperature is 850 ~ 1050 DEG C, heat-insulation pressure keeping 15 ~ 30 minutes, cooling release.
2. the high temperature and high pressure preparation process of Emission in Cubic lanthanum iron titanium oxide according to claim 1, it is characterized in that, described obtained precursor, butyl (tetra) titanate is joined in mass concentration 95% ethanol, produce white precipitate, drip concentrated nitric acid wherein to dissolve completely to precipitation, obtain butyl (tetra) titanate clear solution; By La (NO
3)
3with Fe (NO
3)
3be dissolved in deionized water, then add glucose or the citric acid of butyl (tetra) titanate clear solution and 4.6 ~ 4.9 times of butyl (tetra) titanate mole numbers, stir and be warming up to 70 DEG C, constant temperature is stirred to solution and becomes thickness formation colloidal sol, and rebake obtains dry bulk colloid; 3 hours are sintered, obtained precursor by 500 DEG C, colloid.
3. the high temperature and high pressure preparation process of Emission in Cubic lanthanum iron titanium oxide according to claim 2, is characterized in that, described baking, can be at 110 DEG C dry 24 hours.
4. the high temperature and high pressure preparation process of Emission in Cubic lanthanum iron titanium oxide according to claim 1 and 2, is characterized in that, described HP-HT synthesize, be synthesis pressure is 5GPa, and synthesis temperature is 950 DEG C, heat-insulation pressure keeping 15 minutes.
5. the high temperature and high pressure preparation process of Emission in Cubic lanthanum iron titanium oxide according to claim 1 and 2, is characterized in that, described lanthanum nitrate, iron nitrate, butyl (tetra) titanate are raw material, their quality purity >=99.9%.
6. the product that the high temperature and high pressure preparation process of the Emission in Cubic lanthanum iron titanium oxide of claim 1 is obtained, its component is La
2feTiO
6, structure is cubic structure.
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|---|---|---|---|---|
| CN106243664A (en) * | 2016-08-27 | 2016-12-21 | 南京理工大学 | Ferrum/nitrogen-doped titanic acid lanthanio infrared composite material and preparation method thereof |
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| CN102897845A (en) * | 2012-11-07 | 2013-01-30 | 吉林大学 | High-temperature and high-pressure preparation method for cubic phase barium-iron-antimony oxide |
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2014
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| CN1524792A (en) * | 2003-02-28 | 2004-09-01 | 新加坡纳米材料科技有限公司 | Method for preparing crystalline state perovskite compounds powder |
| CN101293200A (en) * | 2008-05-30 | 2008-10-29 | 内蒙古大学 | Method for preparing dual-perovskite type methyl hydride combustion catalyst containing titanium |
| CN102897845A (en) * | 2012-11-07 | 2013-01-30 | 吉林大学 | High-temperature and high-pressure preparation method for cubic phase barium-iron-antimony oxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243664A (en) * | 2016-08-27 | 2016-12-21 | 南京理工大学 | Ferrum/nitrogen-doped titanic acid lanthanio infrared composite material and preparation method thereof |
| CN106243664B (en) * | 2016-08-27 | 2017-12-12 | 南京理工大学 | Iron/nitrogen-doped titanic acid lanthanum base infrared composite material and preparation method thereof |
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