CN103449536B - Preparation method of perovskite type nano Nd1-xMgxCoO3 - Google Patents
Preparation method of perovskite type nano Nd1-xMgxCoO3 Download PDFInfo
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- CN103449536B CN103449536B CN201310387111.8A CN201310387111A CN103449536B CN 103449536 B CN103449536 B CN 103449536B CN 201310387111 A CN201310387111 A CN 201310387111A CN 103449536 B CN103449536 B CN 103449536B
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Abstract
The invention relates to a preparation method of a perovskite type material, in particular to a preparation method of perovskite type nano Nd1-xMgxCoO3. The method comprises the following steps: preparing precursor of perovskite type Nd1-xMgxCoO3 by taking Nd2O3, Mg(NO3)2, Co(NO3)3.6H2O, NaOH and Na2CO3 as starting materials by a co-precipitation method; calcining the precursor to obtain the perovskite type nano Nd1-xMgxCoO3. The preparation method has the advantages of readily available raw materials, simpler preparation process, safety, no need of large-sized special equipment, less investment, lower production cost, short production period of products, high efficiency and high purity; the particle diameter of the perovskite type nano Nd1-xMgxCoO3 is mainly distributed between 100 nm and 200 nm; the perovskite type nano Nd1-xMgxCoO3 has better industrial utilization prospect.
Description
Technical field
The present invention relates to a kind of preparation method of perovskite type material, be specifically related to a kind of Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method.
Background technology
Perovskite (or uhligite) shaped material belongs to trigonal system, and basic structure is ABO
3, this structure only has when the positively charged ion on A ion position is (as Ca
2+) onesize or larger than it with oxonium ion, and B ion is (as Ti
4+) ligancy be only when being 6 stable, the radius namely between ion meets R
a+ R
o=2
0.5(R
b+ R
o).But meet the extremely few of this ideal situation in real crystal, the crystal of most Perovskite-type structure is not ideal crystal and has certain distortion, and the radius namely between ion meets R
a+ R
o=t2
0.5(R
b+ R
o) (generally t=0.7-1.0).Perovskite type material has this special structure just, 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 the aspect such as sensor, stopper, light micromotor, memory device, matrix or substrate, catalysis electrode, photoelectric device, gas phase separation film, fuel cell.And nanometer perovskite type 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 mechanics, calorifics, magnetics, optics, electricity, acoustics a series of with common polycrystalline body with the essential distinction of non-crystalline solids.And adopt the method for low cost to prepare nanometer perovskite type material to be the key realizing nano material widespread adoption, to be also current problem demanding prompt solution.
Summary of the invention
The invention provides a kind of co-precipitation-sintering process simple, with low cost to prepare Perovskite-type nanometer Nd
1-xmg
xcoO
3.Described method is simple to operation, needs equipment few, and invest little, production cost is low, and efficiency is high, and products obtained therefrom purity is high, has good industrial utilization prospect.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method, comprise the following steps:
(1) according to Nd
1-xmg
xcoO
3middle metallic element ratio, takes the Nd of certain mol proportion
2o
3, Mg (NO
3)
26H
2o and Co (NO
3)
36H
2o; Described x=0 ~ 0.5;
(2) by Co (NO
3)
36H
2o and Mg (NO
3)
26H
2o mixing is fully dissolved with a certain amount of distilled water, makes to obtain Co (NO
3)
3concentration is 0.01 ~ 0.05molL
-1solution A; Meanwhile, by Nd
2o
3add a certain amount of dilute nitric acid dissolution, make to obtain Nd
2o
3concentration is 0.01 ~ 0.025molL
-1solution B;
(3) by A and B mixing also ultrasonic disperse 10 ~ 15min, mixed solution A+B is obtained;
(4) by a certain amount of NaOH and Na
2cO
3add in distilled water respectively, and prepare 0.2 ~ 0.3 molL respectively after ultrasonic wave dissolving 10 ~ 15 min
-1naOH solution and 0.2 ~ 0.3 molL
-1na
2cO
3solution, then pours this NaOH solution into Na
2cO
3mixed solution C is prepared in solution; Described NaOH and Na
2cO
3mol ratio be 1:0.5;
(5) C is added in A+B, make NaOH, Na
2cO
3the two amount of substance and with Co (NO
3)
36H
2the ratio of O amount of substance is 6 ~ 7:1, and leaves standstill filtration after ultrasonic 30 ~ 50min, is precipitated sample D;
(6) with distilled water wash sample D, be neutral rear suction filtration to washings, then use washing with alcohol filter cake again, then by filter cake dry 8 ~ 10h under 100 ~ 150 DEG C of conditions, finally dry cake is fully ground to form meal, obtain Nd
1-xmg
xcoO
3presoma;
(7) by Nd
1-xmg
xcoO
3presoma is placed in heating unit, with 1 ~ 3 DEG C of min
-1temperature rise rate be heated to 800 ~ 900 DEG C insulation 4.0 ~ 6.0h after, Temperature fall is cooled to room temperature, obtains Perovskite-type nanometer Nd
1-xmg
xcoO
3.
According to above-mentioned Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method, step (1) described certain mol proportion is (1-x)/2:x:1.
According to above-mentioned Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method, the described dust technology concentration of step (2) is 0.10 ~ 0.20molL
-1.
According to above-mentioned Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method, the described NaOH solution concentration of step (4) is 2.4 molL
-1, described Na
2cO
3strength of solution is 2.4 molL
-1.
According to above-mentioned Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method, the described presoma meal of step (6) is 200 orders.
According to above-mentioned Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method, the described washings neutrality of step (6) is pH6.8 ~ 7.0.
positive beneficial effect of the present invention:
The raw materials used wide material sources of the present invention, cheap; The inventive method is simple to operation, safety, and equipment is few, invests little, easily produces; Life cycle of the product is short, and efficiency is high, and cost is low, and purity is high, the Perovskite-type nanometer Nd of preparation
1-xmg
xcoO
3particle diameter be mainly distributed between 100 ~ 200nm, there is good industrial utilization prospect.
Accompanying drawing explanation
Fig. 1 is Perovskite-type nanometer Nd prepared by the embodiment of the present invention 1
1-xmg
xcoO
3scanning electron microscope (SEM) picture.
Fig. 2, Fig. 3, Fig. 4 and Fig. 5 are respectively Perovskite-type nanometer Nd prepared by the embodiment of the present invention 1,2,3,4
1-xmg
xcoO
3x-ray powder diffraction (XRD) collection of illustrative plates.
Embodiment
The present invention is set forth further below in conjunction with specific embodiment.Test method in following embodiment, if no special instructions, is ordinary method; Test materials used in following embodiment and reagent, if no special instructions, all purchased from conventional chemical reagent shop.
embodiment 1
The present embodiment Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method, comprise the following steps:
(1) x=0, according to Nd
1-xmg
xcoO
3metallic element ratio, take Nd
2o
36.72g(0.02mol) and Co (NO
3)
36H
2o 14.12g(0.04mol);
(2) by Co (NO
3)
36H
2o 0.8 L distilled water fully dissolves, and makes to obtain Co (NO
3)
3concentration is 0.05molL
-1solution A; Meanwhile, by Nd
2o
3add 1L 0.20molL
-1dilute nitric acid dissolution, makes to obtain Nd
2o
3concentration is 0.02molL
-1solution B;
(3) by A and B mixing also ultrasonic disperse 10min, mixed solution A+B is obtained;
(4) by NaOH6.4g(0.16mol) and Na
2cO
38.48g(0.08mol) add respectively in 0.67L and 0.33L distilled water, and prepare 0.24 molL respectively after ultrasonic wave dissolving 10min
-1naOH solution and 0.24 molL
-1na
2cO
3solution, then pours this NaOH solution into Na
2cO
3mixed solution C is prepared in solution;
(5) C is added in A+B, and after ultrasonic 30min, leave standstill and filter, be precipitated sample D;
(6) with distilled water wash sample D, be neutral (pH is 6.8 ~ 7.0) suction filtration afterwards to washings, then use washing with alcohol filter cake again, then by filter cake dry 8h under 120 DEG C of conditions, finally dry cake is fully ground to form 200 order meals, obtain Nd
1-xmg
xcoO
3presoma;
(7) by Nd
1-xmg
xcoO
3presoma is placed in heating unit, with 3 DEG C of min
-1temperature rise rate be heated to 800 DEG C insulation 6.0h, Temperature fall is cooled to room temperature, obtains Perovskite-type nanometer Nd
1-xmg
xcoO
3;
Gained Perovskite-type nanometer Nd
1-xmg
xcoO
3(x=0) the very high (see figure 2) of purity, its particle diameter is mainly distributed in (see figure 1) between 140 ~ 200nm.
embodiment 2
The present embodiment Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method, comprise the following steps:
(1) x=0.5; According to Nd
1-xmg
xcoO
3metallic element ratio, take Nd
2o
33.36g(0.01mol), Mg (NO
3)
26H
2o 5.12g(0.02mol) and Co (NO
3)
36H
2o 14.12g(0.04mol);
(2) by Co (NO
3)
36H
2o and Mg (NO
3)
26H
2o mixing is fully dissolved with a certain amount of distilled water, makes to obtain Co (NO
3)
3concentration is 0.03molL
-1solution A; Meanwhile, by Nd
2o
3add a certain amount of 0.10molL
-1dilute nitric acid dissolution, makes to obtain Nd
2o
3concentration is 0.025molL
-1solution B;
(3) by A and B mixing also ultrasonic disperse 15min, mixed solution A+B is obtained;
(4) by a certain amount of NaOH and Na
2cO
3add in distilled water respectively, and prepare 0.2 molL respectively after ultrasonic wave dissolving 15min
-1naOH solution and 0.2molL
-1na
2cO
3solution, then pours this NaOH solution into Na
2cO
3prepare mixed solution C in solution, get NaOH and Na
2cO
3mol ratio be 1:0.5;
(5) C is added in A+B, make NaOH and Na
2cO
3with Co (NO
3)
36H
2the mol ratio of O is 7:1, and after ultrasonic 50min, leaves standstill and filter, be precipitated sample D;
(6) with distilled water wash sample D, be neutral (pH is 6.8 ~ 7.0) suction filtration afterwards to washings, then use washing with alcohol filter cake again, then by filter cake dry 8h under 150 DEG C of conditions, finally dry cake is fully ground to form 150 order meals, obtain Nd
1-xmg
xcoO
3presoma;
(7) by Nd
1-xmg
xcoO
3presoma is placed in heating unit, with 1 DEG C of min
-1temperature rise rate be heated to 900 DEG C insulation 5.0h, Temperature fall is cooled to room temperature, obtains Perovskite-type nanometer Nd
1-xmg
xcoO
3;
Gained Perovskite-type nanometer Nd
1-xmg
xcoO
3(x=0.5) the very high (see figure 3) of purity, its particle diameter is mainly distributed between 130 ~ 180nm.
embodiment 3
The present embodiment Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method, comprise the following steps:
(1) x=0.2; According to Nd
1-xmg
xcoO
3metallic element ratio, take Nd
2o
35.38g(0.016mol), Mg (NO
3)
26H
2o 2.05g(0.008mol) and Co (NO
3)
36H
2o 14.12g(0.04mol);
(2) by Co (NO
3)
36H
2o and Mg (NO
3)
26H
2o mixing is fully dissolved with a certain amount of distilled water, makes to obtain Co (NO
3)
3concentration is 0.02molL
-1solution A; Meanwhile, by Nd
2o
3add a certain amount of 0.15molL
-1dilute nitric acid dissolution, makes to obtain Nd
2o
3concentration is 0.015molL
-1solution B;
(3) by A and B and ultrasonic disperse 13min, mixed solution A+B is obtained;
(4) by a certain amount of NaOH and Na
2cO
3add in distilled water respectively, and prepare 0.3 molL respectively after ultrasonic wave dissolving 13min
-1naOH and 0.3molL
-1na
2cO
3solution, then pours this NaOH solution into Na
2cO
3prepare mixed solution C in solution, get NaOH and Na
2cO
3mol ratio be 1:0.5;
(5) C is added in A+B, make NaOH and Na
2cO
3with Co (NO
3)
36H
2the mol ratio of O is 6:1, and after ultrasonic 40min, leaves standstill and filter, be precipitated sample D;
(6) with distilled water wash sample D, be neutral (pH is 6.8 ~ 7.0) suction filtration afterwards to washings, then use washing with alcohol filter cake again, then by filter cake dry 10h under 100 DEG C of conditions, finally dry cake is fully ground to form 250 order meals, obtain Nd
1-xmg
xcoO
3presoma;
(7) by Nd
1-xmg
xcoO
3presoma is placed in heating unit, with 2 DEG C of min
-1temperature rise rate be heated to 900 DEG C insulation 4.0h, Temperature fall is cooled to room temperature, obtains Perovskite-type nanometer Nd
1-xmg
xcoO
3;
Gained Perovskite-type nanometer Nd
1-xmg
xcoO
3(x=0.2) the very high (see figure 4) of purity, its particle diameter is mainly distributed between 130 ~ 180nm.
embodiment 4
The present embodiment Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method, comprise the following steps:
(1) x=0.1; According to Nd
1-xmg
xcoO
3metallic element ratio, take Nd
2o
36.06g(0.018mol), Mg (NO
3)
26H
2o 1.02g(0.004mol) and Co (NO
3)
36H
2o 14.12g(0.04mol);
(2) by Co (NO
3)
36H
2o and Mg (NO
3)
26H
2o mixing is fully dissolved with a certain amount of distilled water, makes to obtain Co (NO
3)
3concentration is 0.01molL
-1solution A; Meanwhile, by Nd
2o
3add a certain amount of 0.20molL
-1dilute nitric acid dissolution, makes to obtain Nd
2o
3concentration is 0.01molL
-1solution B;
(3) by A and B mixing also ultrasonic disperse 12min, mixed solution A+B is obtained;
(4) by a certain amount of NaOH and Na
2cO
3add in distilled water respectively, and prepare 0.25 molL respectively after ultrasonic wave dissolving 13min
-1naOH solution and 0.25 molL
-1na
2cO
3solution, then pours this NaOH solution into Na
2cO
3prepare mixed solution C in solution, get NaOH and Na
2cO
3mol ratio be 1:0.5;
(5) C is added in A+B, make NaOH and Na
2cO
3with Co (NO
3)
36H
2the mol ratio of O is 7:1, and after ultrasonic 45min, leaves standstill and filter, be precipitated sample D;
(6) with distilled water wash sample D, be neutral (pH is 6.8 ~ 7.0) suction filtration afterwards to washings, then use washing with alcohol filter cake again, then by filter cake dry 9h under 130 DEG C of conditions, finally dry cake is fully ground to form 200 order meals, obtain Nd
1-xmg
xcoO
3presoma;
(7) by Nd
1-xmg
xcoO
3presoma is placed in heating unit, with 2 DEG C of min
-1temperature rise rate be heated to 800 DEG C insulation 5.0h, Temperature fall is cooled to room temperature, obtains Perovskite-type nanometer Nd
1-xmg
xcoO
3;
Gained Perovskite-type nanometer Nd
1-xmg
xcoO
3(x=0.1) the very high (see figure 5) of purity, its particle diameter is mainly distributed between 100 ~ 160nm.
The present invention is not limited to above-mentioned embodiment, and those skilled in the art also can make multiple change accordingly, but to be anyly equal to the present invention or similar change all should be encompassed in the scope of the claims in the present invention.
Claims (4)
1. a Perovskite-type nanometer Nd
1-xmg
xcoO
3preparation method, it is characterized in that, comprise the following steps:
(1) according to Nd
1-xmg
xcoO
3middle metallic element ratio, takes the Nd of mol ratio (1-x)/2:x:1
2o
3, Mg (NO
3)
26H
2o and Co (NO
3)
36H
2o; Described x=0 ~ 0.5;
(2) by Co (NO
3)
36H
2o and Mg (NO
3)
26H
2o mixing is fully dissolved with a certain amount of distilled water, makes to obtain Co (NO
3)
3concentration is 0.01 ~ 0.05molL
-1solution A; Meanwhile, by Nd
2o
3add a certain amount of dilute nitric acid dissolution, make to obtain Nd
2o
3concentration is 0.01 ~ 0.025molL
-1solution B;
(3) by A and B mixing also ultrasonic disperse 10 ~ 15min, mixed solution A+B is obtained;
(4) by a certain amount of NaOH and Na
2cO
3add in distilled water respectively, and prepare 0.2 ~ 0.3 molL respectively after ultrasonic wave dissolving 10 ~ 15 min
-1naOH solution and 0.2 ~ 0.3 molL
-1na
2cO
3solution, then pours this NaOH solution into Na
2cO
3mixed solution C is prepared in solution; Described NaOH and Na
2cO
3mol ratio be 1:0.5;
(5) C is added in A+B, make NaOH, Na
2cO
3the two amount of substance and with Co (NO
3)
36H
2the ratio of O amount of substance is 6 ~ 7:1, and leaves standstill filtration after ultrasonic 30 ~ 50min, is precipitated sample D;
(6) with distilled water wash sample D, be neutral rear suction filtration to washings, then use washing with alcohol filter cake again, then by filter cake dry 8 ~ 10h under 100 ~ 150 DEG C of conditions, finally dry cake is fully ground to form meal, obtain Nd
1-xmg
xcoO
3presoma;
(7) by Nd
1-xmg
xcoO
3presoma is placed in heating unit, with 1 ~ 3 DEG C of min
-1temperature rise rate be heated to 800 ~ 900 DEG C insulation 4.0 ~ 6.0h after, Temperature fall is cooled to room temperature, obtains Perovskite-type nanometer Nd
1-xmg
xcoO
3.
2. Perovskite-type nanometer Nd according to claim 1
1-xmg
xcoO
3preparation method, it is characterized in that: the described dust technology concentration of step (2) is 0.10 ~ 0.20molL
-1.
3. Perovskite-type nanometer Nd according to claim 1
1-xmg
xcoO
3preparation method, it is characterized in that: step (6) presoma meal is 200 orders.
4. Perovskite-type nanometer Nd according to claim 1
1-xmg
xcoO
3preparation method, it is characterized in that: step (6) described washings neutrality is pH6.8 ~ 7.0.
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