CN104591722A - Perovskite-type nanometer material and preparation method thereof - Google Patents
Perovskite-type nanometer material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a perovskite-type nanometer material and a preparation method thereof. The preparation method comprises the steps of preparing a precursor of a nanometer (CaxNd1-x)0.1La0.9Co0.5Fe0.5O3(x=0.1-0.4) material from initial raw materials including Nd(NO3)3.6H2O, Ca(NO3)2.4H2O, La(NO3)3.6H2O, Co(NO3)3.6H2O and Fe(NO3)3.6H2O by using a coprecipitation method; and calcining the precursor to obtain the nanometer (CaxNd1-x) 0.1La0.9Co0.5Fe0.5O3(x=0.1-0.4) material. The preparation method disclosed by the invention has the advantages that the raw materials are available; the preparation method is simple and safe in step, free of large special equipment, small in investment and relatively low in production cost; and the product is short in production period, high in purity, stable in structure, resistant to chemical corrosion and relatively good in industrial application prospect.
Description
Technical field
The present invention relates to a kind of nano material, be specifically related to a kind of calcium-titanium ore type nano material and preparation method thereof.
Background technology
Perovskite-type material belongs to trigonal system, and basic structure is ABO
3(A and B represents positively charged ion, and O represents oxonium ion).Up to now, the oxide compound ABO with perovskite structure is found
3three kinds of ionic radius of type compound meet following relationship: R
a+ R
o=t2
0.5(R
b+ R
o) (generally t=0.7 ~ 1.0).Because perofskite type oxide material has this special structure, perovskite-type material is made to have much special character, as thermoelectricity capability, superconductivity, piezoelectric property, optical property, magnetic performance etc.Improve again the performance of perovskite-type material by doping in practical application, can say that perovskite-type material is a kind of extremely important functional materials, be of wide application, as catalysis, fuel cell, sensor, stopper, light micromotor, memory device, matrix or the aspect such as substrate, photoelectric device.And nano-perovskite shaped material has unique nanocrystal and high-density Grain Boundary Character and the surface effects produced therefrom, small-size effect and macro quanta tunnel effect, it is made to show at aspect of performances such as chemistry, mechanics, calorifics, magnetics, optics, electricity, acoustics a series of with common polycrystalline body with the essential distinction of non-crystalline solids.
Chinese patent CN103449536A discloses a kind of Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method, adopt metallic cation instead of uhligite ABO
3play the A position metal ion of supporting structure skeleton in type composite oxide material, cause larger lattice distortion, improve the performance such as its catalysis and chemistry.
Summary of the invention
The object of the present invention is to provide a kind of calcium-titanium ore type nano material, molecular formula is (Ca
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3, x=0.1 ~ 0.4 in formula.
Another object of the present invention is also the preparation method providing a kind of calcium-titanium ore type nano material, and step is simple, safely, without the need to large-scale specific installation, less investment, production cost is lower, and life cycle of the product is short, and product purity is high.
For achieving the above object, the present invention adopts following technical scheme:
A kind of calcium-titanium ore type nano material, described calcium-titanium ore type nano material molecular formula is (Ca
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3, x=0.1 ~ 0.4 in formula.
A preparation method for above-mentioned calcium-titanium ore type nano material, comprises the following steps:
(1) a certain amount of Nd is dissolved with distilled water respectively
(nO
3 ) 36H
2o, Ca (NO
3)
24H
2o, La (NO
3)
36H
2o, Co (NO
3)
36H
2o, Fe
2(SO
4)
39H
2o, is mixed with Nd respectively
(nO
3 ) 3, Ca (NO
3)
2, La (NO
3)
3, Co (NO
3)
3and Fe
2(SO
4)
3concentration is 0.2 ~ 0.5 molL
-1solution;
(2) according to (Ca
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3metallic element ratio in material, by step (1) a certain amount of Nd
(nO
3 ) 3, Ca (NO
3)
2, La (NO
3)
3, Co (NO
3)
3and Fe
2(SO
4)
3solution mixes, and ultrasonic disperse 8 ~ 15 min, obtains mixed solution A;
(3) be 0.20 ~ 0.30 molL by concentration
-1kOH solution and concentration are 0.05 ~ 0.15 molL
-1k
2cO
3solution is 1 ~ 3:1 mixing by volume, obtains solution B;
(4) solution B is dropwise added in solution A, stir, ultrasonic disperse 30 ~ 60 min, pH value to solution is 10 ~ 11, then centrifugation 3 ~ 5 min, collecting precipitation, adopts distilled water wash precipitation, until washing is to neutral rear suction filtration, then use dissolve with ethanol filter cake, after continuing ultrasonic disperse 10 ~ 20 min, then carry out centrifugation 3 ~ 5min, so 3 ~ 5 times repeatedly, be precipitated sample C;
(5) deposit sample C is placed in baking oven and dries 12 ~ 24 h under 100 ~ 110 DEG C of conditions, finally the material of oven dry is fully ground to form meal, obtain (Ca
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3(x=0.1 ~ 0.4) presoma D, described x=0.1 ~ 0.4;
(6) presoma D is placed in electric furnace, with 5 ~ 10 DEG C of min
-1temperature rise rate be heated to 450 ~ 500 DEG C of insulation 1.0 ~ 3.0 h after, then with 3 ~ 6 DEG C of min
-1temperature rise rate continue to be heated to 800 ~ 900 DEG C of insulation 2.0 ~ 4.0 h after, Temperature fall is cooled to room temperature, obtains nanometer (Nd
xca
1-x)
0.1la
0.9co
0.5fe
0.5o
3material, described x=0.1 ~ 0.4.
According to the preparation method of above-mentioned calcium-titanium ore type nano material, the baking oven described in step (5) is blast dry oven.
According to the preparation method of above-mentioned calcium-titanium ore type nano material, the nanometer (Ca described in step (6)
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3material particle size is 80 ~ 120 nm.
positive beneficial effect of the present invention:
(1) the present invention adopts other metallic cations to instead of uhligite ABO
3play the A position metal ion of main support structure skeleton in type composite oxide material, cause larger lattice distortion, improve the performance such as its catalysis and chemistry; Be on the basis replaced at A, other transition-metal cations are adopted again to instead of the B position ion of the functions such as main catalytic active, prepare the perovskite-type material with that A position and B position replace and that there is mixed valence structure, make this material system energy larger, only need can there is the transformation that electronic structure matches under less energy drives, thus obtain the performances such as more excellent magnetics, optics, electricity, surface and catalysis.
(2) perovskite typed nanometer (Ca of the present invention
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3material adopts A position and B position ion to replace the oxide perovskite material of replacement simultaneously, has the feature of ionic valence condition in a big way in modulation and control texture and lattice defect, can keep good thermodynamic stability again simultaneously.
(3) the raw materials used wide material sources of the present invention, cheap; Preparation method of the present invention, simple to operation, safety, equipment is few, invests little, easily produces; Life cycle of the product is short, and cost is low, and purity is high, and particle diameter is 80 ~ 120 nm, Stability Analysis of Structures, resistance to chemical attack, has good industrial utilization prospect.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the X-ray diffraction of the embodiment of the present invention 1 calcium-titanium ore type nano material;
Fig. 2 is the XRD figure spectrum of the X-ray diffraction of the embodiment of the present invention 2 calcium-titanium ore type nano material;
Fig. 3 is the XRD figure spectrum of the X-ray diffraction of the embodiment of the present invention 3 calcium-titanium ore type nano material.
Embodiment
Below in conjunction with some specific embodiments, the present invention is further described.
Embodiment 1
A kind of calcium-titanium ore type nano material, described calcium-titanium ore type nano material molecular formula is (Ca
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3, x=0.4 in formula.
Above-mentioned perovskite typed nanometer (Ca
0.4nd
0.6)
0.1la
0.9co
0.5fe
0.5o
3the preparation method of material, comprises the following steps:
(1) Nd of 21.9120g is weighed
(nO
3 ) 36H
2ca (the NO of O, 11.8075g
3)
24H
2la (the NO of O, 21.6500g
3)
36H
2co (the NO of O, 17.6500g
3)
36H
2the Fe of O, 28.1005g
2(SO
4)
39H
2o, then adding a certain amount of distilled water respectively, to be mixed with concentration be respectively 0.5 molL
-1nd
(nO
3 ) 3, Ca (NO
3)
2, La (NO
3)
3, Co (NO
3)
3and Fe
2(SO
4)
3solution;
(2) according to (Ca
0.4nd
0.6)
0.1la
0.9co
0.5fe
0.5o
3metallic element stoichiometric ratio (Ca:Nd:La:Co:Fe=0.04:0.06:0.9:0.5:0.5) in material, respectively by the Ca (NO of above-mentioned steps (1) gained 4ml
3)
2the Nd of solution, 6ml
(nO
3 ) 3la (the NO of solution, 90ml
3)
3co (the NO of solution, 50ml
3)
3the Fe of solution, 25ml
2(SO
4)
3solution mixes, and obtains mixed solution A after ultrasonic disperse mixing 10min;
(3) by 0.30 molL
-1kOH solution and concentration be 0.15 molL
-1k
2cO
3solution be by volume 2:1 mixing, obtain solution B;
(4) solution B is dropwise added in solution A, stir, ultrasonic disperse 60 min, pH value to solution is 10, then centrifugation 5 min, collecting precipitation, adopts distilled water wash precipitation, until washing is to neutral rear suction filtration, then use dissolve with ethanol filter cake, after continuing ultrasonic disperse 20 min, then carry out centrifugation 5 min, so 3 times repeatedly, be precipitated sample C;
(5) deposit sample C is placed in baking oven and dries 20 h under 110 DEG C of conditions, finally the material of oven dry is fully ground to form meal, obtain ((Ca
0.4nd
0.6)
0.1la
0.9co
0.5fe
0.5o
3presoma D;
(6) presoma D is placed in electric furnace, with 5 DEG C of min
-1temperature rise rate be heated to 500 DEG C insulation 3 h after, then with
3 DEG C of min
-1temperature rise rate continue to be heated to 800 DEG C of insulation 2.0 h after, Temperature fall is cooled to room temperature, obtains nanometer (Ca
0.4nd
0.6)
0.1la
0.9co
0.5fe
0.5o
3material.
As can be seen from Figure 1, product (Ca
0.4nd
0.6)
0.1la
0.9co
0.5fe
0.5o
3the purity of perovskite material is high, and be single uhligite crystalline phase, median size is 80 nm, and feed stock conversion is 99%.
embodiment 2
A kind of calcium-titanium ore type nano material, described calcium-titanium ore type nano material molecular formula is (Ca
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3, x=0.3 in formula.
Above-mentioned perovskite typed nanometer (Ca
0.3nd
0.7)
0.1la
0.9co
0.5fe
0.5o
3the preparation method of material, comprises the following steps:
(1) Nd (NO of 17.5296g is first weighed
3)
36H
2ca (the NO of O, 9.4460g
3)
24H
2la (the NO of O, 17.3200g
3)
36H
2co (the NO of O, 14.1200g
3)
36H
2the Fe of O, 22.4804g
2(SO
4)
39H
2o, then adding a certain amount of distilled water respectively, to be mixed with concentration be respectively 0.4 molL
-1nd
(nO
3 ) 3, Ca (NO
3)
2, La (NO
3)
3, Co (NO
3)
3and Fe
2(SO
4)
3solution;
(2) according to (Ca
0.3nd
0.7)
0.1la
0.9co
0.5fe
0.5o
3metallic element stoichiometric ratio (Ca:Nd:La:Co:Fe=0.03:0.07:0.9:0.5:0.5) in material, respectively by the Ca (NO of above-mentioned steps (1) gained 3ml
3)
2nd (the NO of solution, 7ml
3)
3la (the NO of solution, 90ml
3)
3co (the NO of solution, 50ml
3)
3the Fe of solution, 25ml
2(SO
4)
3solution) mixing, ultrasonic disperse mixing 8min, obtains mixed solution A;
(3) by 0.20 molL
-1kOH and 0.05 molL
-1k
2cO
3volume ratio be 3:1 mixing, obtain solution B;
(4) solution B is dropwise added in solution A, stir, ultrasonic disperse 50 min, pH value to solution is 11, then centrifugation 4 min, collecting precipitation, adopts distilled water wash precipitation, until washing is to neutral rear suction filtration, then use dissolve with ethanol filter cake, after continuing ultrasonic disperse 15 min, then carry out centrifugation 4 min, so 4 times repeatedly, be precipitated sample C;
(5) deposit sample C is placed in convection oven and dries 12 h under 100 DEG C of conditions, finally the material of oven dry is fully ground to form meal, obtain (Ca
0.3nd
0.7)
0.1la
0.9co
0.5fe
0.5o
3presoma D;
(6) presoma D is placed in electric furnace, with 8 DEG C of min
-1temperature rise rate be heated to 450 DEG C of insulation 2 h after, then with 4 DEG C of min
-1temperature rise rate continue to be heated to 820 DEG C of insulation 4.0 h after, Temperature fall is cooled to room temperature, obtains nanometer (Ca
0.3nd
0.7)
0.1la
0.9co
0.5fe
0.5o
3material.
As can be seen from Figure 2, product (Ca
0.3nd
0.7)
0.1la
0.9co
0.5fe
0.5o
3the purity of perovskite material is high, and be single uhligite crystalline phase, median size is 100 nm, and feed stock conversion is 100%.
embodiment 3
A kind of calcium-titanium ore type nano material, described calcium-titanium ore type nano material molecular formula is (Ca
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3, x=0.1 in formula.
Above-mentioned perovskite typed nanometer (Ca
0.1nd
0.9)
0.1la
0.9co
0.5fe
0.5o
3the preparation method of material, comprises the following steps:
(1) Nd of 17.5296g is first weighed
(nO
3 ) 36H
2ca (the NO of O, 9.4460g
3)
24H
2la (the NO of O, 17.3200g
3)
36H
2co (the NO of O, 14.1200g
3)
36H
2the Fe of O, 22.4804g
2(SO
4)
39H
2o, then adding a certain amount of distilled water respectively, to be mixed with concentration be respectively 0.2 molL
-1nd
(nO
3 ) 3, Ca (NO
3)
2, La (NO
3)
3, Co (NO
3)
3and Fe
2(SO
4)
3solution;
(2) according to (Ca
0.1nd
0.9)
0.1la
0.9co
0.5fe
0.5o
3metallic element stoichiometric ratio (Ca:Nd:La:Co:Fe=0.01:0.09:0.9:0.5:0.5) in material, respectively by the Ca (NO of above-mentioned steps (1) gained 2ml
3)
2nd (the NO of solution, 18 ml
3)
3la (the NO of solution, 180 ml
3)
3co (the NO of solution, 100 ml
3)
3the Fe of solution, 50 ml
2(SO
4)
3solution mixes, and ultrasonic disperse 15 min, obtains mixed solution A;
(3) by 0.20 molL
-1kOH and 0.10 molL
-1k
2cO
3volume ratio be 1:1 mixing, obtain solution B;
(4) solution B is dropwise added in solution A, stir, ultrasonic disperse 30 min, pH value to solution is 11, then centrifugation 3 min, collecting precipitation, adopts distilled water wash precipitation, until washing is to neutral rear suction filtration, then use dissolve with ethanol filter cake, after continuing ultrasonic disperse 10 min, then carry out centrifugation 3 min, so 5 times repeatedly, be precipitated sample C;
(5) deposit sample C is placed in convection oven and dries 24h under 110 DEG C of conditions, finally the material of oven dry is fully ground to form meal, obtain (Ca
0.1nd
0.9)
0.1la
0.9co
0.5fe
0.5o
3presoma D;
(6) presoma D is placed in electric furnace, with 10 DEG C of min
-1temperature rise rate be heated to 460 DEG C of insulation 1 h after, then with 6 DEG C of min
-1temperature rise rate continue to be heated to 900 DEG C of insulation 3.0 h after, Temperature fall is cooled to room temperature, obtains nanometer (Ca
0.1nd
0.9)
0.1la
0.9co
0.5fe
0.5o
3material.
As can be seen from Figure 3, product (Ca
0.1nd
0.9)
0.1la
0.9co
0.5fe
0.5o
3the purity of perovskite material is very high, and be single uhligite crystalline phase, median size is 120 nm, and feed stock conversion is 99%.
Claims (4)
1. a calcium-titanium ore type nano material, is characterized in that, described calcium-titanium ore type nano material molecular formula is (Ca
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3, x=0.1 ~ 0.4 in formula.
2. a preparation method for calcium-titanium ore type nano material according to claim 1, is characterized in that, comprises the following steps:
(1) a certain amount of Nd (NO is dissolved with distilled water respectively
3 ) 36H
2o, Ca (NO
3)
24H
2o, La (NO
3)
36H
2o, Co (NO
3)
36H
2o, Fe
2(SO
4)
39H
2o, is mixed with Nd (NO respectively
3 ) 3, Ca (NO
3)
2, La (NO
3)
3, Co (NO
3)
3and Fe
2(SO
4)
3concentration is 0.2 ~ 0.5molL
-1solution;
(2) according to (Ca
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3metallic element stoichiometric ratio in material, by a certain amount of for step (1) Nd (NO
3 ) 3, Ca (NO
3)
2, La (NO
3)
3, Co (NO
3)
3and Fe
2(SO
4)
3solution mixes, and ultrasonic disperse 8 ~ 15 min, obtains mixed solution A;
(3) be 0.20 ~ 0.30 molL by concentration
-1kOH solution and concentration are 0.05 ~ 0.15 molL
-1k
2cO
3solution is 1 ~ 3:1 mixing by volume, obtains solution B;
(4) solution B is dropwise added in solution A, stir, ultrasonic disperse 30 ~ 60 min, pH value to solution is 10 ~ 11, then centrifugation 3 ~ 5 min, collecting precipitation, adopts distilled water wash precipitation, until washing is to neutral rear suction filtration, then use dissolve with ethanol filter cake, after continuing ultrasonic disperse 10 ~ 20 min, then carry out centrifugation 3 ~ 5min, so 3 ~ 5 times repeatedly, be precipitated sample C;
(5) deposit sample C is placed in baking oven and dries 12 ~ 24 h under 100 ~ 110 DEG C of conditions, finally the material of oven dry is fully ground to form meal, obtain (Ca
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3presoma D, described x=0.1 ~ 0.4;
(6) presoma D is placed in electric furnace, with 5 ~ 10 DEG C of min
-1temperature rise rate be heated to 450 ~ 500 DEG C of insulation 1.0 ~ 3.0 h after, then with 3 ~ 6 DEG C of min
-1temperature rise rate continue to be heated to 800 ~ 900 DEG C of insulation 2.0 ~ 4.0 h after, Temperature fall is cooled to room temperature, obtains nanometer (Nd
xca
1-x)
0.1la
0.9co
0.5fe
0.5o
3material, described x=0.1 ~ 0.4.
3. the preparation method of calcium-titanium ore type nano material according to claim 2, is characterized in that, the baking oven described in step (5) is blast dry oven.
4. the preparation method of calcium-titanium ore type nano material according to claim 2, is characterized in that, the nanometer (Ca described in step (6)
xnd
1-x)
0.1la
0.9co
0.5fe
0.5o
3material particle size is 80 ~ 120 nm.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107857301A (en) * | 2017-11-09 | 2018-03-30 | 东南大学 | A kind of calcium swage Ca2Fe2O5Method for preparing catalyst |
CN112844391A (en) * | 2021-01-13 | 2021-05-28 | 宁夏大学 | Perovskite type multi-metal composite oxygen carrier and preparation method thereof |
CN114011425A (en) * | 2021-12-08 | 2022-02-08 | 湘潭大学 | Bifunctional catalyst, preparation method, application and application method thereof |
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CN101746834A (en) * | 2009-12-19 | 2010-06-23 | 山西大学 | Preparation method of perovskite composite oxide La1-xCaxFeO3 superfines |
CN102142564A (en) * | 2011-02-24 | 2011-08-03 | 安徽工业大学 | LaFeO3-base cathode material of sulfur-oxygen fuel cell |
CN102751508A (en) * | 2011-04-19 | 2012-10-24 | 三星电子株式会社 | Cathode material for a fuel cell, cathode including the cathode material, and a solid oxide fuel cell including the cathode material |
CN103449536A (en) * | 2013-08-30 | 2013-12-18 | 华北水利水电大学 | Preparation method of perovskite type nano Nd1-xMgxCoO3 |
-
2015
- 2015-01-05 CN CN201510002279.1A patent/CN104591722B/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101746834A (en) * | 2009-12-19 | 2010-06-23 | 山西大学 | Preparation method of perovskite composite oxide La1-xCaxFeO3 superfines |
CN102142564A (en) * | 2011-02-24 | 2011-08-03 | 安徽工业大学 | LaFeO3-base cathode material of sulfur-oxygen fuel cell |
CN102751508A (en) * | 2011-04-19 | 2012-10-24 | 三星电子株式会社 | Cathode material for a fuel cell, cathode including the cathode material, and a solid oxide fuel cell including the cathode material |
CN103449536A (en) * | 2013-08-30 | 2013-12-18 | 华北水利水电大学 | Preparation method of perovskite type nano Nd1-xMgxCoO3 |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107857301A (en) * | 2017-11-09 | 2018-03-30 | 东南大学 | A kind of calcium swage Ca2Fe2O5Method for preparing catalyst |
CN112844391A (en) * | 2021-01-13 | 2021-05-28 | 宁夏大学 | Perovskite type multi-metal composite oxygen carrier and preparation method thereof |
CN114011425A (en) * | 2021-12-08 | 2022-02-08 | 湘潭大学 | Bifunctional catalyst, preparation method, application and application method thereof |
CN114011425B (en) * | 2021-12-08 | 2023-12-05 | 湘潭大学 | Dual-function catalyst and preparation method and application method thereof |
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