CN108178183A - A kind of La doped strontium titanate nano powder and preparation method thereof - Google Patents
A kind of La doped strontium titanate nano powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of La doped strontium titanate nano powder and preparation method thereof, the molecular formula of La doped strontium titanate nano powder is LaxSr(1‑x)TiO3, and preparation method includes the following steps：S1, solution A is prepared；S2, solution B is prepared；S3, solution C is prepared；S4, solution A, solution B and solution C are mixed to prepare solution D；S5, solution D react and calcine obtained white puff powder；S6, La doped strontium titanate nano powder is made.Compared with prior art, the beneficial effects of the invention are as follows：La doped strontium titanates is nano-scale and is perovskite structure；The preparation method process of the present invention is simple, easy to operate, raw material it is cheap, product rate is high, can be widely used in the preparation of industrial production and laboratory nan powder；Reaction spontaneous can carry out, and save the energy, reduce reaction temperature, save the reaction time.
Description
Technical field
The invention belongs to field of thermoelectric material technique, more particularly to a kind of La doped strontium titanate nano powder and its preparation side
Method.
Background technology
With the development of modern science and technology, energy and environmental problem becomes increasingly conspicuous, thermoelectric material is as novel energy material day
Benefit is valued by people.Thermoelectric material, which does not need to other movable parts, can be directly realized by mutual turn of thermal energy and electric energy
It changes, for thermo-electric generation and thermoelectric cooling.Since thermo-electric generation and refrigeration system have small, simple in structure, the noiseless, longevity
The advantages that life is long, safe and reliable, has broad application prospects in cogeneration etc..Oxide pyroelectric material is because of some
Unique advantage is in recent years as one of important research direction of thermoelectric material, with other kinds of oxide pyroelectric material phase
Than strontium titanate base thermoelectric ceramic material is because with typical perovskite structure, and carrier effective mass (m*) is than tradition half
Big two orders of magnitude of conductor thermoelectric material have vast potential for future development in high-temperature oxide thermoelectric material field.At present, have perhaps
More means are used to improve the thermoelectricity capability of material, wherein, element doping is one of most common means, and many studies have shown that receiving
The structure of rice structure has the performance of block thermoelectric material apparent improvement result.Lanthanum is that strontium titanate base thermoelectric material is the most frequently used
Doped chemical.
Invention content
The object of the present invention is to provide a kind of La doped strontium titanate nano powders and preparation method thereof.
The preparation method of the present invention uses lanthanum nitrate (La (NO3)3·6H2O), strontium nitrate (Sr (NO3)2), butyl titanate (Ti
(OC4H9)4) as lanthanum source, barium source and titanium source, using citric acid as fuel, synthesis required temperature is relatively low, it is shorter to be spent between inverse time,
And the grain size of La doped strontium titanate nano powder prepared is Nano grade.
To achieve these goals, the technical solution that the application uses for：
A kind of La doped strontium titanate nano powder, the molecular formula of the La doped strontium titanate nano powder is LaxSr(1-x)
TiO3, wherein 0.1≤x ﹤ 1.
Further, the molecular formula of the La doped strontium titanate nano powder is La0.1Sr0.9TiO3。
A kind of preparation method of La doped strontium titanate nano powder, includes the following steps：S1, solution A is prepared；S2, preparation
Solution B；S3, solution C is prepared；S4, solution A, solution B and solution C are mixed to prepare solution D；S5, solution D are reacted and are calcined obtained
White puff powder；S6, La doped strontium titanate nano powder is made；Wherein,
S1, the process of preparation solution A are as follows：
By Ti (OC4H9)4It is added dropwise in the deionized water being stirred continuously, generates a large amount of white precipitates；Then 30wt% is added dropwise
Nitric acid, and stir after white precipitate dissolving after, it is static, remove a layer solution；The lemon that finally lower floor's solution inflow is stirred continuously
In lemon acid solution, obtained solution A；Wherein, the ratio between amount of substance of the citric acid in the citric acid solution and titanium elements is
1.5:1；
S2, the process of preparation solution B are as follows：
Soluble lanthanum salt is dissolved in citric acid solution, obtained solution B；Wherein, the lemon in the citric acid solution
The ratio between acid and the amount of substance of lanthanum element are 1.5:1；
S3, the process of preparation solution C are as follows：
Soluble strontium salt is dissolved in citric acid solution, obtained solution C；Wherein, the lemon in the citric acid solution
The ratio between acid and the amount of substance of strontium element are 1.5:1；
S4, solution A, solution B and solution C are mixed evenly, obtained solution D；
S5, first, the pH for adjusting solution D are 7；Then, the solution D that pH is 7 is heated simultaneously under the conditions of 75 DEG C~85 DEG C
Stirring, obtains brownish red gel；Finally, 1.5h~2.5h, system are calcined under the conditions of brownish red gel being placed in 600 DEG C~700 DEG C
Obtain white puff powder；
S6, by after the white puff powder nitric acid filtering and washing 3~5 times of 0.8mol/L~1.2mol/L, 75 DEG C~
La doped strontium titanate nano powder is dried to obtain at a temperature of 85 DEG C.
Further, in S1, the Ti (OC of 0.8moL~1.2moL are dissolved in 1400mL~2000mL deionized waters4H9)4。
Further, the mass fraction of the citric acid solution is 50%.
Further, in S2, soluble lanthanum salt is La (NO3)3﹒ 6H2In O, S3, soluble strontium salt is Sr (NO3)2。
Compared with prior art, beneficial effects of the present invention：
(1) this La doped strontium titanate nano powder grain size is Nano grade, and grain size is evenly distributed；
(2) preparation process of the invention is easy to operate, raw material it is cheap, product rate is high, can be widely used in industry
Production and the preparation of laboratory nan powder；
(3) involved in preparation process of the invention to chemical reaction be exothermic reaction, it can be ensured that reaction it is spontaneous into
Row, not only saves the energy, but also greatly reduce reaction temperature, saves the reaction time.
Description of the drawings
Fig. 1 is the XRD spectrum of La doped strontium titanate nano powder prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM spectrum of La doped strontium titanate nano powder prepared by the embodiment of the present invention 1；
Fig. 3 is the EDS collection of illustrative plates of La doped strontium titanate nano powder prepared by the embodiment of the present invention 1；
Fig. 4 is only to change the SEM of La doped strontium titanate nano powder figures prepared by the pH of solution D in the embodiment of the present invention 1
Spectrum；
Specific embodiment
In order to make the present invention technological means, creation characteristic, achieving the goal is easy to understand with effect, below in conjunction with
Technical scheme of the present invention is clearly and completely described in the embodiment of the present invention.
Embodiment 1
Molecular formula is La0.1Sr0.9TiO3La doped strontium titanate nano powder.
The preparation method of above-mentioned La doped strontium titanate nano powder, including step following six：
S1, solution A is prepared：
First, the butyl titanate Ti (OC of the i.e. 1moL of 340.32g are weighed4H9)4Being stirred continuously into 1400mL is slowly added dropwise
Deionized water in, until no white precipitate generate until；Then, the nitric acid of 30wt% is added in, and is stirred continuously to white
It is static after precipitation is completely dissolved, remove a layer solution；Finally, it in citric acid solution lower floor's solution inflow being stirred continuously, is made
Solution A；Wherein, the citric acid in citric acid solution and titanyl nitrate TiO (NO3)4The ratio between amount of substance of middle titanium elements is 1.5:
1, and the mass fraction of citric acid solution is 50%；
The process for preparation of above-mentioned citric acid solution is：The citric acid for weighing 288.2g, that is, 1.5moL is dissolved in 288.2mL's
In deionized water, citric acid and titanyl nitrate TiO (NO are obtained3)4The ratio between amount of substance of middle titanium elements is 1.5:1, and quality point
Number is 50% citric acid solution；
S2, solution B is prepared：
Weigh 43.3g i.e. 0.1moL lanthanum nitrate hexahydrates La (NO3)3﹒ 6H2O is dissolved in citric acid solution, obtained solution
B；Wherein, the citric acid in citric acid solution and lanthanum nitrate hexahydrate La (NO3)3﹒ 6H2The ratio between amount of substance of lanthanum element in O
It is 1.5:1, and the mass fraction of citric acid solution is 50%；
The process for preparation of above-mentioned citric acid solution is：The citric acid for weighing 28.8g, that is, 0.15moL is dissolved in going for 28.8mL
In ionized water, citric acid and lanthanum nitrate hexahydrate La (NO are obtained3)3﹒ 6H2The ratio between amount of substance of lanthanum element in O is 1.5:1,
And the citric acid solution that mass fraction is 50%；
S3, the process of preparation solution C are as follows：
Weigh 190.5g i.e. 0.9moL strontium nitrates Sr (NO3)2It is dissolved in citric acid solution, obtained solution C；Wherein, lemon
Citric acid and strontium nitrate Sr (NO in acid solution3)2The ratio between amount of substance of middle strontium element is 1.5:1, and the matter of citric acid solution
It is 50% to measure score；
The process for preparation of above-mentioned citric acid solution is：The citric acid for weighing 259.4g, that is, 1.35moL is dissolved in 259.4mL's
In deionized water, citric acid and strontium nitrate Sr (NO are obtained3)2The ratio between amount of substance of middle strontium element is 1.5:1, and mass fraction
For 50% citric acid solution；
S4, solution A, solution B and solution C are mixed evenly, obtained solution D；
S5, first, the pH for adjusting solution D are 7；Then, the solution D that pH is 7 is heated and stirred in 80 DEG C of waters, obtained
To brownish red gel；Finally, brownish red gel is placed in 650 DEG C of Muffle furnace, calcines 2h, white puff powder is made；
It is S6, dry by after the white puff powder nitric acid filtering and washing 4 times of 1mol/L, then at a temperature of 80 DEG C
To La doped strontium titanate nano powder.
Embodiment 2
Molecular formula is La0.4Sr0.5TiO3La doped strontium titanate nano powder.
The preparation method of above-mentioned La doped strontium titanate nano powder, including step following six：
S1, solution A is prepared：
First, the butyl titanate Ti (OC of the i.e. 1moL of 340.32g are weighed4H9)4Being stirred continuously into 1600mL is slowly added dropwise
Deionized water in, until no white precipitate generate until；Then, then the nitric acid of 30wt% is added dropwise, and be stirred continuously to white
It is static after color precipitation is completely dissolved, remove a layer solution；Finally, in citric acid solution lower floor's solution inflow being stirred continuously, system
Obtain solution A；Wherein, the citric acid in citric acid solution and titanyl nitrate TiO (NO3)4The ratio between amount of substance of middle titanium elements is
1.5:1, and the mass fraction of citric acid solution is 50%；
The process for preparation of above-mentioned citric acid solution is：The citric acid for weighing 288.2g, that is, 1.5moL is dissolved in 288.2mL's
In deionized water, citric acid and titanyl nitrate TiO (NO are obtained3)4The ratio between amount of substance of middle titanium elements is 1.5:1, and quality point
Number is 50% citric acid solution；
S2, solution B is prepared：
Weigh 173.2g i.e. 0.4moL lanthanum nitrate hexahydrates La (NO3)3﹒ 6H2O is dissolved in citric acid solution, obtained solution
B；Wherein, the citric acid in citric acid solution and lanthanum nitrate hexahydrate La (NO3)3﹒ 6H2The ratio between amount of substance of lanthanum element in O
It is 1.5:1, and the mass fraction of citric acid solution is 50%；
The process for preparation of above-mentioned citric acid solution is：The citric acid for weighing 115.3g, that is, 0.6moL is dissolved in 115.3mL's
In deionized water, citric acid and lanthanum nitrate hexahydrate La (NO are obtained3)3﹒ 6H2The ratio between amount of substance of lanthanum element in O is 1.5:
1, and the citric acid solution that mass fraction is 50%；
S3, the process of preparation solution C are as follows：
Weigh 105.8g i.e. 0.5moL strontium nitrates Sr (NO3)2It is dissolved in citric acid solution, obtained solution C；Wherein, lemon
Citric acid and strontium nitrate Sr (NO in acid solution3)2The ratio between amount of substance of middle strontium element is 1.5:1, and the matter of citric acid solution
It is 50% to measure score；
The process for preparation of above-mentioned citric acid solution is：The citric acid for weighing 144.2g, that is, 0.75moL is dissolved in 144.2mL's
In deionized water, citric acid and strontium nitrate Sr (NO are obtained3)2The ratio between amount of substance of middle strontium element is 1.5:1, and mass fraction
For 50% citric acid solution；
S4, solution A, solution B and solution C are mixed evenly, obtained solution D；
S5, first, the pH for adjusting solution D are 7；Then, the solution D that pH is 7 is heated and stirred in 75 DEG C of waters, obtained
To brownish red gel；Finally, brownish red gel is placed in 600 DEG C of Muffle furnace, calcines 1.5h, white puff powder is made；
It is S6, dry by after the white puff powder nitric acid filtering and washing 5 times of 0.8mol/L, then at a temperature of 75 DEG C
Obtain La doped strontium titanate nano powder.
Embodiment 3
Molecular formula is La0.9Sr0.1TiO3La doped strontium titanate nano powder.
The preparation method of above-mentioned La doped strontium titanate nano powder, including step following six：
S1, solution A is prepared：
First, the butyl titanate Ti (OC of the i.e. 1moL of 340.32g are weighed4H9)4Being stirred continuously into 2000mL is slowly added dropwise
Deionized water in, until no white precipitate generate until；The nitric acid of 30wt% is added dropwise again, and is stirred continuously to white precipitate
It is static after being completely dissolved, remove a layer solution；Finally, in citric acid solution lower floor's solution inflow being stirred continuously, obtained solution
A；Wherein, the citric acid in citric acid solution and titanyl nitrate TiO (NO3)4The ratio between amount of substance of middle titanium elements is 1.5:1, and
The mass fraction of citric acid solution is 50%；
The process for preparation of above-mentioned citric acid solution is：The citric acid for weighing 288.2g, that is, 1.5moL is dissolved in 288.2mL's
In deionized water, citric acid and titanyl nitrate TiO (NO are obtained3)4The ratio between amount of substance of middle titanium elements is 1.5:1, and quality point
Number is 50% citric acid solution；
S2, solution B is prepared：
Weigh 389.7g i.e. 0.9moL lanthanum nitrate hexahydrates La (NO3)3﹒ 6H2O is dissolved in citric acid solution, obtained solution
B；Wherein, the citric acid in citric acid solution and lanthanum nitrate hexahydrate La (NO3)3﹒ 6H2The ratio between amount of substance of lanthanum element in O
It is 1.5:1, and the mass fraction of citric acid solution is 50%；
The process for preparation of above-mentioned citric acid solution is：The citric acid for weighing 259.4g, that is, 1.35moL is dissolved in 259.4mL's
In deionized water, citric acid and lanthanum nitrate hexahydrate La (NO are obtained3)3﹒ 6H2The ratio between amount of substance of lanthanum element in O is 1.5:
1, and the citric acid solution that mass fraction is 50%；
S3, the process of preparation solution C are as follows：
Weigh 21.2g i.e. 0.1moL strontium nitrates Sr (NO3)2It is dissolved in citric acid solution, obtained solution C；Wherein, lemon
Citric acid and strontium nitrate Sr (NO in acid solution3)2The ratio between amount of substance of middle strontium element is 1.5:1, and the matter of citric acid solution
It is 50% to measure score；
The process for preparation of above-mentioned citric acid solution is：The citric acid for weighing 28.8g, that is, 0.15moL is dissolved in going for 28.8mL
In ionized water, citric acid and strontium nitrate Sr (NO are obtained3)2The ratio between amount of substance of middle strontium element is 1.5:1, and mass fraction is
50% citric acid solution；
S4, solution A, solution B and solution C are mixed evenly, obtained solution D；
S5, first, the pH for adjusting solution D are 7；Then, the solution D that pH is 7 is heated and stirred in 85 DEG C of waters, obtained
To brownish red gel；Finally, brownish red gel is placed in 700 DEG C of Muffle furnace, calcines 2.5h, white puff powder is made；
It is S6, dry by after the white puff powder nitric acid filtering and washing 3 times of 1.2mol/L, then at a temperature of 85 DEG C
Obtain La doped strontium titanate nano powder.
In order to further detect the performance of the La doped strontium titanate nano powder prepared by the embodiment of the present invention 1~3, we
By taking material is prepared in embodiment 1 as an example, it is tested for the property and analyzes, particular content is as follows：
Wherein Fig. 1-Fig. 3 is respectively La0.1Sr0.9TiO3XRD spectra, SEM spectrograms and EDS spectrograms.
By Fig. 1 it can be seen that La0.1Sr0.9TiO3Characteristic peak and perovskite structure strontium titanates characteristic peak quantity
It is identical, and position is close, compared to the characteristic peak of the strontium titanates of perovskite structure, the characteristic peak of La doped strontium titanates of the invention
It is only the offset having occurred slightly.Features above can illustrate the La doped strontium titanates being prepared by the method for the present invention
La0.1Sr0.9TiO3Nano-powder is perovskite structure, and lanthanum element is doped into strontium titanates really.
Even more intuitively see that La doped strontium titanates prepared by the present invention is perovskite structure, and grain size is about by Fig. 2
20nm illustrates through the La doped strontium titanates of La doped strontium titanates prepared by the present invention for Nano grade.
It is further proved by Fig. 3 in nano-powder prepared by the present invention containing lanthanum element, strontium element, titanium elements and oxygen
Element illustrates that lanthanum element is successfully doped in strontium titanates, and nano-powder is the La of pure free from admixture0.1Sr0.9TiO3Nanometer
Powder.
This method uses low-temperature combustion synthesis, explores the reasonable process ginseng for effectively preparing La doped strontium titanate base powder
Number.Compared in thermoelectric ceramics precursor powder preparation method apply more conventional solid reaction method, preparation method of the invention
High performance doping precursor powder can be directly obtained by reaction, and powder size is nanoscale, and conventional solid reaction method
The powder being prepared is micron order.The preparation method of the present invention is simple for process, and the period is short, yield is big, energy consumption is small.
If Fig. 4 is only changes the pH in embodiment 1, the SEM spectrum of the La doped strontium titanate nano powder of preparation, from Fig. 4
In it is found that only in pH=7, the structure for the nano-powder being prepared is only perovskite structure.So also it shows that the present invention
In the preparation method for preparing La doped strontium titanate nano powder, only in the range of the technological parameter of the present invention, can just it prepare
Perovskite structure and Nano grade La doped Sr titanate powder.
In conclusion beneficial effects of the present invention：
(1) not only Nano grade, grain size are evenly distributed the grain size of La doped Sr titanate powder prepared by the present invention, and
Powder structure is perovskite structure；
(2) preparation process of the invention is easy to operate, raw material it is cheap, product rate is high, can be widely used in industry
Production and the preparation of laboratory nan powder；
(3) involved in preparation process of the invention to chemical reaction be exothermic reaction, it can be ensured that reaction it is spontaneous into
Row, not only saves the energy, but also greatly reduce reaction temperature, saves the reaction time.
Disclosed above is only presently preferred embodiments of the present invention, and still, the embodiment of the present invention is not limited to this, Ren Heben
What the technical staff in field can think variation should all fall into protection scope of the present invention.
Claims (6)
1. a kind of La doped strontium titanate nano powder, the molecular formula of the La doped strontium titanate nano powder is LaxSr(1-x)TiO3,
Wherein 0.1≤x ﹤ 1.
2. a kind of La doped strontium titanate nano powder as described in claim 1, which is characterized in that the La doped strontium titanates is received
The molecular formula of rice flour body is La0.1Sr0.9TiO3。
3. the preparation method of a kind of La doped strontium titanate nano powder as described in right 1 or 2, which is characterized in that including as follows
Step：S1, solution A is prepared；S2, solution B is prepared；S3, solution C is prepared；S4, solution A, solution B and solution C are mixed to prepare molten
Liquid D；S5, solution D react and calcine obtained white puff powder；S6, La doped strontium titanate nano powder is made；Wherein,
S1, the process of preparation solution A are as follows：
By Ti (OC4H9)4It is added dropwise in the deionized water being stirred continuously, generates a large amount of white precipitates；Then the nitre of 30wt% is added dropwise
Acid, and stir after white precipitate dissolving, it is static, remove a layer solution；The citric acid that finally lower floor's solution inflow is stirred continuously
In solution, obtained solution A；Wherein, the ratio between amount of substance of the citric acid in the citric acid solution and titanium elements is 1.5:1；
S2, the process of preparation solution B are as follows：
Soluble lanthanum salt is dissolved in citric acid solution, obtained solution B；Wherein, the citric acid in the citric acid solution with
The ratio between amount of substance of lanthanum element is 1.5:1；
S3, the process of preparation solution C are as follows：
Soluble strontium salt is dissolved in citric acid solution, obtained solution C；Wherein, the citric acid in the citric acid solution with
The ratio between amount of substance of strontium element is 1.5:1；
S4, solution A, solution B and solution C are mixed evenly, obtained solution D；
S5, first, the pH for adjusting solution D are 7；Then, the solution D that pH is 7 is heated and stirred under the conditions of 75 DEG C~85 DEG C,
Obtain brownish red gel；Finally, 1.5h~2.5h is calcined under the conditions of brownish red gel being placed in 600 DEG C~700 DEG C, white is made
Fluffy powder；
S6, by after the white puff powder nitric acid filtering and washing 3~5 times of 0.8mol/L~1.2mol/L, at 75 DEG C~85 DEG C
At a temperature of be dried to obtain La doped strontium titanate nano powder.
4. a kind of preparation method of La doped strontium titanate nano powder as claimed in claim 3, which is characterized in that in S1,
Ti (the OC of 0.8moL~1.2moL are dissolved in 1400mL~2000mL deionized waters4H9)4。
A kind of 5. preparation method of La doped strontium titanate nano powder as claimed in claim 3, which is characterized in that the lemon
The mass fraction of acid solution is 50%.
6. a kind of preparation method of La doped strontium titanate nano powder as claimed in claim 3, which is characterized in that, can in S2
Dissolubility lanthanum salt is La (NO3)3·6H2O；In S3, soluble strontium salt is Sr (NO3)2。
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| 常文博: "SOFC镧掺杂钛酸锶阳极材料制备及电极性能的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110065618A (en) * | 2019-03-25 | 2019-07-30 | 西北工业大学 | A kind of multifunction structure device and its working method for hypersonic aircraft |
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| CN108178183B (en) | 2020-01-10 |
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