CN108178183B - Lanthanum-doped strontium titanate nano powder and preparation method thereof - Google Patents
Lanthanum-doped strontium titanate nano powder and preparation method thereof Download PDFInfo
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- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000011858 nanopowder Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 13
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 291
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 229910052746 lanthanum Inorganic materials 0.000 claims description 13
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 13
- 239000010936 titanium Substances 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- 229910052712 strontium Inorganic materials 0.000 claims description 10
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 150000002603 lanthanum Chemical class 0.000 claims description 4
- 159000000008 strontium salts Chemical class 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 239000002105 nanoparticle Substances 0.000 abstract 1
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 20
- 239000000463 material Substances 0.000 description 11
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 6
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 4
- GJKFIJKSBFYMQK-UHFFFAOYSA-N lanthanum(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GJKFIJKSBFYMQK-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- PXRKCOCTEMYUEG-UHFFFAOYSA-N 5-aminoisoindole-1,3-dione Chemical compound NC1=CC=C2C(=O)NC(=O)C2=C1 PXRKCOCTEMYUEG-UHFFFAOYSA-N 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 description 3
- DQTJHJVUOOYAMD-UHFFFAOYSA-N oxotitanium(2+) dinitrate Chemical compound [O-][N+](=O)O[Ti](=O)O[N+]([O-])=O DQTJHJVUOOYAMD-UHFFFAOYSA-N 0.000 description 3
- 238000010248 power generation Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- -1 0.75moL Chemical compound 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
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Abstract
The invention discloses lanthanum-doped strontium titanate nano powder and a preparation method thereof, wherein the molecular formula of the lanthanum-doped strontium titanate nano powder is LaxSr(1‑x)TiO3The preparation method comprises the following steps: s1, preparing a solution A; s2, preparing a solution B; s3, preparing a solution C; s4, mixing the solution A, the solution B and the solution C to obtain a solution D; s5, reacting the solution D and calcining to obtain white fluffy powder; s6, preparing the lanthanum-doped strontium titanate nano powder. Compared with the prior art, the invention has the beneficial effects that: the lanthanum-doped strontium titanate is nano-sized and has a perovskite structure; the preparation method has simple process, easy operation, low price of raw materials and high product yield, and can be widely applied to industrial production and preparation of laboratory nano powder; the reaction can be carried out spontaneously, so that the energy is saved, the reaction temperature is reduced, and the reaction time is saved.
Description
Technical Field
The invention belongs to the technical field of thermoelectric materials, and particularly relates to lanthanum-doped strontium titanate nano powder and a preparation method thereof.
Background
With the development of modern science and technology, the problems of energy and environment are increasingly prominent, and the thermoelectric material is increasingly paid attention to as a novel energy material. The thermoelectric material can directly realize the interconversion of heat energy and electric energy without other movable parts, and is used for thermoelectric power generation and thermoelectric refrigeration. The thermoelectric power generation and refrigeration system has the advantages of small volume, simple structure, no noise, long service life, safety, reliability and the like, and has wide application prospect in the aspects of waste heat power generation and the like. Compared with other types of oxide thermoelectric materials, the strontium titanate-based thermoelectric ceramic material has a typical perovskite structure, the carrier effective mass (m) of the strontium titanate-based thermoelectric ceramic material is two orders of magnitude larger than that of the traditional semiconductor thermoelectric material, and the strontium titanate-based thermoelectric ceramic material has a wide development prospect in the field of high-temperature oxide thermoelectric materials. At present, there are many means for improving the thermoelectric properties of materials, wherein element doping is one of the most common means, and many studies show that the construction of nanostructures has a significant improvement effect on the properties of bulk thermoelectric materials. Lanthanum is the most commonly used doping element for strontium titanate based thermoelectric materials.
Disclosure of Invention
The invention aims to provide lanthanum-doped strontium titanate nano powder and a preparation method thereof.
The preparation method adopts lanthanum nitrate (La (NO)3)3·6H2O), strontium nitrate (Sr (NO)3)2) Butyl titanate (Ti (OC)4H9)4) As a lanthanum source, a strontium source and a titanium source, citric acid is used as a fuel, the temperature required by synthesis is low, the reverse time is short, and the particle size of the prepared lanthanum-doped strontium titanate nano powder is in a nano level.
In order to achieve the purpose, the technical scheme adopted by the application is as follows:
lanthanum-doped strontium titanate nano powder, wherein the molecular formula of the lanthanum-doped strontium titanate nano powder is LaxSr(1-x)TiO3Wherein x is more than or equal to 0.1 and less than 1.
Furthermore, the molecular formula of the lanthanum-doped strontium titanate nano powder is La0.1Sr0.9TiO3。
A preparation method of lanthanum-doped strontium titanate nano powder comprises the following steps: s1, preparing a solution A; s2, preparing a solution B; s3, preparing a solution C; s4, mixing the solution A, the solution B and the solution C to obtain a solution D; s5, reacting the solution D and calcining to obtain white fluffy powder; s6, preparing lanthanum-doped strontium titanate nano powder; wherein,
s1, the process for preparing solution A is as follows:
mixing Ti (OC)4H9)4Dripping into deionized water under stirring to generate a large amount of white precipitate; then 30 wt% nitric acid is added dropwise and stirred to whiteAfter dissolving the precipitate, standing, and taking the lower layer solution; finally, enabling the lower-layer solution to flow into a citric acid solution which is continuously stirred to prepare a solution A; wherein the amount ratio of citric acid to titanium in the citric acid solution is 1.5: 1;
s2, the process for preparing the solution B is as follows:
dissolving soluble lanthanum salt in a citric acid solution to prepare a solution B; wherein the mass ratio of citric acid to lanthanum in the citric acid solution is 1.5: 1;
s3, the process for preparing solution C is as follows:
dissolving soluble strontium salt in a citric acid solution to prepare a solution C; wherein the mass ratio of citric acid to strontium in the citric acid solution is 1.5: 1;
s4, mixing and stirring the solution A, the solution B and the solution C uniformly to obtain a solution D;
s5, firstly, adjusting the pH value of the solution D to 7; then, heating and stirring the solution D with the pH value of 7 at the temperature of 75-85 ℃ to obtain a brownish red gel; finally, calcining the brownish red gel for 1.5 to 2.5 hours at the temperature of between 600 and 700 ℃ to prepare white fluffy powder;
s6, carrying out suction filtration and washing on the white fluffy powder for 3-5 times by using 0.8-1.2 mol/L nitric acid, and drying at the temperature of 75-85 ℃ to obtain the lanthanum-doped strontium titanate nano powder.
Further, in S1, 0.8 moL-1.2 moL of Ti (OC) is dissolved in 1400 mL-2000 mL of deionized water4H9)4。
Further, the citric acid solution is 50% by mass.
Further, in S2, the soluble lanthanum salt is La (NO)3)3∙6H2In O, S3, the soluble strontium salt is Sr (NO)3)2。
Compared with the prior art, the invention has the beneficial effects that:
(1) the lanthanum-doped strontium titanate nano powder has nano-grade grain diameter and uniform grain diameter size distribution;
(2) the preparation process of the invention is easy to operate, the raw materials are low in price, the product yield is high, and the preparation method can be widely applied to industrial production and preparation of laboratory nano powder;
(3) the chemical reaction involved in the preparation process of the invention is exothermic reaction, which can ensure the spontaneous proceeding of the reaction, not only save energy, but also greatly reduce the reaction temperature and save the reaction time.
Drawings
FIG. 1 is an XRD pattern of lanthanum-doped strontium titanate nanopowder prepared in example 1 of the present invention;
FIG. 2 is an SEM image of lanthanum-doped strontium titanate nanopowder prepared in example 1 of the invention;
FIG. 3 is an EDS spectrum of lanthanum-doped strontium titanate nanopowder prepared in example 1 of the invention;
FIG. 4 is an SEM image of lanthanum-doped strontium titanate nanopowder prepared by changing only the pH of solution D in example 1 of the present invention;
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the technical scheme of the invention is clearly and completely described below by combining the embodiment of the invention.
Example 1
Molecular formula is La0.1Sr0.9TiO3The lanthanum-doped strontium titanate nano powder.
The preparation method of the lanthanum-doped strontium titanate nano powder comprises the following six steps:
s1, preparation of solution a:
first, 340.32g of 1moL of Ti tetrabutyltitanate (OC) were weighed4H9)4Slowly adding 1400mL of deionized water which is continuously stirred until no white precipitate is generated; then, adding 30 wt% of nitric acid, continuously stirring until the white precipitate is completely dissolved, standing, and taking the lower layer solution; finally, enabling the lower-layer solution to flow into a citric acid solution which is continuously stirred to prepare a solution A; wherein citric acid in the citric acid solution is mixed with TiO (NO) nitrate3)4The ratio of the amount of titanium element in the solution is 1.5:1, and the citric acid solution isThe mass fraction is 50 percent;
the preparation process of the citric acid solution comprises the following steps: 288.2g of 1.5moL citric acid was weighed and dissolved in 288.2mL deionized water to obtain citric acid and titanyl nitrate TiO (NO)3)4Citric acid solution with the mass fraction of 50% and the mass ratio of the titanium element in the citric acid solution being 1.5: 1;
s2, preparation of solution B:
43.3g, i.e. 0.1moL, of La (NO) nitrate hexahydrate are weighed out3)3∙6H2Dissolving O in citric acid solution to obtain solution B; wherein the citric acid in the citric acid solution is mixed with lanthanum nitrate La (NO) hexahydrate3)3∙6H2The mass ratio of lanthanum element in O is 1.5:1, and the mass fraction of the citric acid solution is 50%;
the preparation process of the citric acid solution comprises the following steps: 28.8g, i.e. 0.15moL, of citric acid was weighed out and dissolved in 28.8mL of deionized water to obtain citric acid and lanthanum nitrate hexahydrate La (NO)3)3∙6H2A citric acid solution in which the mass ratio of lanthanum element in O is 1.5:1 and the mass fraction is 50%;
s3, the process for preparing solution C is as follows:
weighing 190.5g of 0.9moL strontium nitrate Sr (NO)3)2Dissolving in citric acid solution to obtain solution C; wherein, citric acid and strontium nitrate Sr (NO) in the citric acid solution3)2The mass ratio of the strontium element in the solution is 1.5:1, and the mass fraction of the citric acid solution is 50%;
the preparation process of the citric acid solution comprises the following steps: 259.4g of 1.35moL of citric acid are weighed and dissolved in 259.4mL of deionized water to obtain citric acid and strontium nitrate Sr (NO)3)2A citric acid solution with the mass fraction of 50% and the mass ratio of strontium elements in the citric acid solution being 1.5: 1;
s4, mixing and stirring the solution A, the solution B and the solution C uniformly to obtain a solution D;
s5, firstly, adjusting the pH value of the solution D to 7; then, heating and stirring the solution D with the pH value of 7 in a water area with the temperature of 80 ℃ to obtain a brownish red gel; finally, placing the brownish red gel in a muffle furnace at 650 ℃, and calcining for 2h to prepare white fluffy powder;
s6, carrying out suction filtration and washing on the white fluffy powder for 4 times by using 1mol/L nitric acid, and drying at the temperature of 80 ℃ to obtain the lanthanum-doped strontium titanate nano powder.
Example 2
Molecular formula is La0.4Sr0.5TiO3The lanthanum-doped strontium titanate nano powder.
The preparation method of the lanthanum-doped strontium titanate nano powder comprises the following six steps:
s1, preparation of solution a:
first, 340.32g of 1moL of Ti tetrabutyltitanate (OC) were weighed4H9)4Slowly adding the mixture into 1600mL of deionized water which is continuously stirred until no white precipitate is generated; then, dropwise adding 30 wt% of nitric acid, continuously stirring until the white precipitate is completely dissolved, standing, and taking the lower layer solution; finally, enabling the lower-layer solution to flow into a citric acid solution which is continuously stirred to prepare a solution A; wherein citric acid in the citric acid solution is mixed with TiO (NO) nitrate3)4The mass ratio of the titanium element in the solution is 1.5:1, and the mass fraction of the citric acid solution is 50%;
the preparation process of the citric acid solution comprises the following steps: 288.2g of 1.5moL citric acid was weighed and dissolved in 288.2mL deionized water to obtain citric acid and titanyl nitrate TiO (NO)3)4Citric acid solution with the mass fraction of 50% and the mass ratio of the titanium element in the citric acid solution being 1.5: 1;
s2, preparation of solution B:
173.2g, i.e. 0.4moL, of La nitrate hexahydrate (NO) are weighed out3)3∙6H2Dissolving O in citric acid solution to obtain solution B; wherein the citric acid in the citric acid solution is mixed with lanthanum nitrate La (NO) hexahydrate3)3∙6H2The mass ratio of lanthanum element in O is 1.5:1, and the mass fraction of the citric acid solution is 50%;
the preparation process of the citric acid solution comprises the following steps: 115.3g, i.e. 0.6moL, of citric acid was weighed out and dissolved in 115.3mL of deionized water,obtaining citric acid and lanthanum nitrate hexahydrate La (NO)3)3∙6H2A citric acid solution in which the mass ratio of lanthanum element in O is 1.5:1 and the mass fraction is 50%;
s3, the process for preparing solution C is as follows:
105.8g of strontium nitrate Sr (NO) of 0.5moL are weighed3)2Dissolving in citric acid solution to obtain solution C; wherein, citric acid and strontium nitrate Sr (NO) in the citric acid solution3)2The mass ratio of the strontium element in the solution is 1.5:1, and the mass fraction of the citric acid solution is 50%;
the preparation process of the citric acid solution comprises the following steps: 144.2g of citric acid, i.e. 0.75moL, was weighed and dissolved in 144.2mL of deionized water to obtain citric acid and strontium nitrate Sr (NO)3)2A citric acid solution with the mass fraction of 50% and the mass ratio of strontium elements in the citric acid solution being 1.5: 1;
s4, mixing and stirring the solution A, the solution B and the solution C uniformly to obtain a solution D;
s5, firstly, adjusting the pH value of the solution D to 7; then, heating and stirring the solution D with the pH value of 7 in a water area with the temperature of 75 ℃ to obtain a brownish red gel; finally, placing the brownish red gel in a muffle furnace at 600 ℃, and calcining for 1.5h to prepare white fluffy powder;
s6, carrying out suction filtration and washing on the white fluffy powder for 5 times by using 0.8mol/L nitric acid, and drying at the temperature of 75 ℃ to obtain the lanthanum-doped strontium titanate nano powder.
Example 3
Molecular formula is La0.9Sr0.1TiO3The lanthanum-doped strontium titanate nano powder.
The preparation method of the lanthanum-doped strontium titanate nano powder comprises the following six steps:
s1, preparation of solution a:
first, 340.32g of 1moL of Ti tetrabutyltitanate (OC) were weighed4H9)4Slowly adding the mixture into 2000mL of deionized water which is continuously stirred until no white precipitate is generated; then 30 wt% nitric acid is added dropwise, and the mixture is continuously stirred until white precipitate is completely dissolved, and then the mixture is staticTaking down the lower layer solution; finally, enabling the lower-layer solution to flow into a citric acid solution which is continuously stirred to prepare a solution A; wherein citric acid in the citric acid solution is mixed with TiO (NO) nitrate3)4The mass ratio of the titanium element in the solution is 1.5:1, and the mass fraction of the citric acid solution is 50%;
the preparation process of the citric acid solution comprises the following steps: 288.2g of 1.5moL citric acid was weighed and dissolved in 288.2mL deionized water to obtain citric acid and titanyl nitrate TiO (NO)3)4Citric acid solution with the mass fraction of 50% and the mass ratio of the titanium element in the citric acid solution being 1.5: 1;
s2, preparation of solution B:
389.7g of 0.9moL lanthanum nitrate hexahydrate La (NO) are weighed3)3∙6H2Dissolving O in citric acid solution to obtain solution B; wherein the citric acid in the citric acid solution is mixed with lanthanum nitrate La (NO) hexahydrate3)3∙6H2The mass ratio of lanthanum element in O is 1.5:1, and the mass fraction of the citric acid solution is 50%;
the preparation process of the citric acid solution comprises the following steps: 259.4g of citric acid, i.e. 1.35moL, were weighed out and dissolved in 259.4mL of deionized water to obtain citric acid and lanthanum nitrate hexahydrate, La (NO)3)3∙6H2A citric acid solution in which the mass ratio of lanthanum element in O is 1.5:1 and the mass fraction is 50%;
s3, the process for preparing solution C is as follows:
21.2g of 0.1moL strontium nitrate Sr (NO) are weighed3)2Dissolving in citric acid solution to obtain solution C; wherein, citric acid and strontium nitrate Sr (NO) in the citric acid solution3)2The mass ratio of the strontium element in the solution is 1.5:1, and the mass fraction of the citric acid solution is 50%;
the preparation process of the citric acid solution comprises the following steps: 28.8g, i.e., 0.15moL, of citric acid was weighed and dissolved in 28.8mL of deionized water to obtain citric acid and strontium nitrate Sr (NO)3)2A citric acid solution with the mass fraction of 50% and the mass ratio of strontium elements in the citric acid solution being 1.5: 1;
s4, mixing and stirring the solution A, the solution B and the solution C uniformly to obtain a solution D;
s5, firstly, adjusting the pH value of the solution D to 7; then, heating and stirring the solution D with the pH value of 7 in a water area at 85 ℃ to obtain a brownish red gel; finally, placing the brownish red gel in a muffle furnace at 700 ℃, and calcining for 2.5h to prepare white fluffy powder;
s6, carrying out suction filtration and washing on the white fluffy powder for 3 times by using 1.2mol/L nitric acid, and drying at the temperature of 85 ℃ to obtain the lanthanum-doped strontium titanate nano powder.
In order to further detect the performance of the lanthanum-doped strontium titanate nano powder prepared in embodiments 1-3 of the present invention, we take the material prepared in embodiment 1 as an example, and perform performance testing and analysis, specifically including the following contents:
wherein FIG. 1-FIG. 3 are La respectively0.1Sr0.9TiO3XRD, SEM and EDS spectra of (A).
La can be seen from FIG. 10.1Sr0.9TiO3The characteristic peaks of the lanthanum-doped strontium titanate of the invention are the same in number and similar in position to the characteristic peaks of the strontium titanate of the perovskite structure, and the characteristic peaks of the lanthanum-doped strontium titanate of the invention are only slightly shifted compared with the characteristic peaks of the strontium titanate of the perovskite structure. The above characteristics can illustrate that lanthanum-doped strontium titanate La prepared by the method of the present invention0.1Sr0.9TiO3The nano powder is in a perovskite structure, and the lanthanum element is really doped into the strontium titanate.
It is more intuitive from fig. 2 that the lanthanum-doped strontium titanate prepared by the present invention has a perovskite structure and a particle size of about 20nm, which indicates that the lanthanum-doped strontium titanate prepared by the present invention is nano-grade lanthanum-doped strontium titanate.
Fig. 3 further shows that the nano-powder prepared by the invention contains lanthanum, strontium, titanium and oxygen, which indicates that lanthanum is successfully doped into strontium titanate, and the nano-powder is pure La without impurities0.1Sr0.9TiO3And (3) nano powder.
The method adopts a low-temperature combustion synthesis method to explore reasonable process parameters for effectively preparing lanthanum-doped strontium titanate-based powder. Compared with the traditional solid-phase reaction method which is applied more in the preparation method of the thermoelectric ceramic precursor powder, the preparation method of the invention can directly obtain the high-performance doped precursor powder through reaction, and the powder size is nano-scale, while the powder prepared by the traditional solid-phase reaction method is micron-scale. The preparation method has the advantages of simple process, short period, high yield and low energy consumption.
As shown in fig. 4, which is an SEM image of the lanthanum-doped strontium titanate nanopowder prepared by changing the pH in example 1, it can be seen from fig. 4 that the structure of the nanopowder prepared is a perovskite structure only when the pH is 7. Therefore, the preparation method for preparing lanthanum-doped strontium titanate nano powder can prepare the lanthanum-doped strontium titanate powder with a perovskite structure and a nano level only within the range of the process parameters of the invention.
In conclusion, the invention has the beneficial effects that:
(1) the lanthanum-doped strontium titanate powder prepared by the method has the advantages that the particle size is not only in a nanometer level, but also is uniform in particle size distribution, and the powder structure is of a perovskite structure;
(2) the preparation process of the invention is easy to operate, the raw materials are low in price, the product yield is high, and the preparation method can be widely applied to industrial production and preparation of laboratory nano powder;
(3) the chemical reaction involved in the preparation process of the invention is exothermic reaction, which can ensure the spontaneous proceeding of the reaction, not only save energy, but also greatly reduce the reaction temperature and save the reaction time.
The above disclosure is only for the preferred embodiments of the present invention, but the embodiments of the present invention are not limited thereto, and any variations that can be made by those skilled in the art are intended to fall within the scope of the present invention.
Claims (4)
1. A preparation method of lanthanum-doped strontium titanate nano powder, wherein the molecular formula of the lanthanum-doped strontium titanate nano powder is LaxSr(1-x)TiO3Wherein x is more than or equal to 0.1 and less than 1, and is characterized by comprising the following steps:
s1, preparing a solution A; s2, preparing a solution B; s3, preparing a solution C; s4, mixing the solution A, the solution B and the solution C to obtain a solution D; s5, reacting the solution D and calcining to obtain white fluffy powder; s6, preparing lanthanum-doped strontium titanate nano powder; wherein,
s1, the process for preparing solution A is as follows:
mixing Ti (OC)4H9)4Dripping into deionized water under stirring to generate a large amount of white precipitate; then dropwise adding 30 wt% of nitric acid, stirring until the white precipitate is dissolved, standing, and taking the lower layer solution; finally, enabling the lower-layer solution to flow into a citric acid solution which is continuously stirred to prepare a solution A; wherein the amount ratio of citric acid to titanium in the citric acid solution is 1.5: 1;
s2, the process for preparing the solution B is as follows:
dissolving soluble lanthanum salt in a citric acid solution to prepare a solution B; wherein the mass ratio of citric acid to lanthanum in the citric acid solution is 1.5: 1;
s3, the process for preparing solution C is as follows:
dissolving soluble strontium salt in a citric acid solution to prepare a solution C; wherein the mass ratio of citric acid to strontium in the citric acid solution is 1.5: 1;
s4, mixing and stirring the solution A, the solution B and the solution C uniformly to obtain a solution D;
s5, firstly, adjusting the pH value of the solution D to 7; then, heating and stirring the solution D with the pH value of 7 at the temperature of 75-85 ℃ to obtain a brownish red gel; finally, calcining the brownish red gel for 1.5 to 2.5 hours at the temperature of between 600 and 700 ℃ to prepare white fluffy powder;
s6, carrying out suction filtration and washing on the white fluffy powder for 3-5 times by using 0.8-1.2 mol/L nitric acid, and drying at the temperature of 75-85 ℃ to obtain the lanthanum-doped strontium titanate nano powder.
2. The method of claim 1, wherein 0.8 moL-1.2 moL of Ti (OC) is dissolved in 1400 mL-2000 mL of deionized water in S14H9)4。
3. The method of claim 1, wherein the citric acid solution is 50% by mass.
4. The method of claim 1, wherein in S2, the soluble lanthanum salt is La (NO)3)3∙6H2O; in S3, the soluble strontium salt is Sr (NO)3)2。
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