CN104556211B - A kind of tin dope solvent thermal-hydro-thermal method prepares Sm2Sn2O7/SnO2The method of nano-complex - Google Patents
A kind of tin dope solvent thermal-hydro-thermal method prepares Sm2Sn2O7/SnO2The method of nano-complex Download PDFInfo
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Abstract
Disclosure one tin dope solvent thermal-hydro-thermal method prepares Sm2Sn2O7/SnO2The method of nano-complex: by SmCl3·6H2O and SnCl4·5H2O is with 1:(0.1～1) mol ratio be dissolved in alcoholic solution obtained solution A；Regulate pH to 7～13 and form reaction precursor liquid；Being poured into by reaction precursor liquid in the hot inner bag of politef, heated sealed, reaction naturally cools to room temperature after terminating；Product washing, dry to obtain Sm2Sn2O7；By the analytical pure SnCl that mass fraction is 2%～5%4·5H2O and Sm2Sn2O7Put into reactor, put into reaction in baking oven after envelope still and naturally cool to room temperature after terminating；Product washing, dry to obtain Sm2Sn2O7/SnO2Nano-complex.Reaction medium of the present invention is that organic solvent is of a great variety, and boiling point is low, can effectively prevent the oxidizing process of product and the pollution of air oxygen, is beneficial to and prepares High Purity compound.
Description
[technical field]
The present invention relates to Nano semiconductor field of composite material preparation, be specifically related to one and prepare Sm2Sn2O7/SnO2The method of nano-complex.
[background technology]
Sm2Sn2O7It is typical rare earth metal pyrochlore constitution material, in lattice, has a lot of function replacement positions.Nano level Sm2Sn2O7With the characteristic of rare earth and nano material, having the performance of uniqueness in optics, electricity, catalysis etc., the novel inorganic functional material in the multiple physical and chemical performances such as ionic conductivity, catalytic, ferroelectric-ferromagnetic has potential using value.
So single Sm2Sn2O7Photocatalysis performance is limited.
[summary of the invention]
It is an object of the invention to provide a kind of tin dope solvent thermal-hydro-thermal method and prepare Sm2Sn2O7/SnO2The method of nano-complex, this reaction medium kind is many, low-boiling organic solution, can effectively prevent the oxidizing process of product and the pollution of air oxygen, being beneficial to and prepare High Purity compound, and reaction raw materials is easy to get, feasibility is strong, process equipment is simple, utilizing magnetic agitation that reaction can be made more full and uniform, it is possible to prepare and have better photocatalytic activity, purity is high, crystallinity is strong, the uniform Sm of pattern2Sn2O7/SnO2Nano-complex.
For reaching above-mentioned purpose, the technical solution used in the present invention is:
A kind of tin dope solvent thermal-hydro-thermal method prepares Sm2Sn2O7/SnO2The method of nano-complex, comprises the following steps:
1) by analytical pure SmCl3·6H2O and SnCl4·5H2O is with 1:(0.1～1) mol ratio be dissolved in solvent prepare Sm3+Concentration is the solution A of 0.0022～0.08mol/L；
2) regulate the pH to 7～13 of solution A, continue stirring 1～2h and form reaction precursor liquid；
3) being poured into by reaction precursor liquid in the hot inner bag of politef, heated sealed, react 10～40h at 100～200 DEG C, reaction naturally cools to room temperature after terminating；
4) product washs, dries, and obtains Sm2Sn2O7；
5) by analytical pure SnCl4·5H2The Sm of O and 0.0242～0.144mol/L2Sn2O7The mixed solution that solution is mixed to form puts into reactor, puts in baking oven after envelope still, reacts 3～5h at 100～200 DEG C, and reaction naturally cools to room temperature after terminating；Added SnCl4·5H2It is 2%～5% that O accounts for the mass fraction of mixed solution；
6) product washs, dries, and obtains Sm2Sn2O7/SnO2Nano-complex.
Described solvent is organic solution.
Step 2) middle employing analytical pure ammonia adjustment pH value.
Step 4) described washing, dry particularly as follows: successively with distilled water and dehydrated alcohol centrifuge washing 4～6 times, collect product vacuum drying 0.5～2h at 60～80 DEG C.
Step 6) described washing, dry particularly as follows: successively with distilled water and dehydrated alcohol centrifuge washing 4～6 times, collect product vacuum drying 0.5～2h at 60～80 DEG C.
Described solvent is ethanol.
Relative to prior art, the method have the advantages that
The present invention prepares Sm with tin dope solvent thermal-hydro-thermal method2Sn2O7/SnO2Nano-complex.By a certain amount of analytical pure SmCl3·6H2O and SnCl4·5H2O is dissolved in ethanol in proper amount solution obtained solution A；Adopt analytical pure ammonia to regulate the pH of solution A, form reaction precursor liquid；Being poured into by reaction precursor liquid in the hot inner bag of politef, heated sealed, reaction naturally cools to room temperature after terminating；Product with distilled water and dehydrated alcohol centrifuge washing, is collected product in vacuum drying, is obtained Sm successively2Sn2O7Product.Analytical pure SnCl by 2%～5% (mass fraction)4·5H2O and a certain amount of Sm2Sn2O7Putting into reactor, put in baking oven and react after envelope still, reaction naturally cools to room temperature after terminating；Product with distilled water and dehydrated alcohol centrifuge washing, is collected product in vacuum drying, is obtained Sm successively2Sn2O7/SnO2Nano-complex.
In the present invention, reaction medium is that organic solvent is of a great variety, and boiling point is low, can effectively prevent the oxidizing process of product and the pollution of air oxygen, is beneficial to and prepares High Purity compound, and reaction raw materials is easy to get, and feasibility is strong, and process equipment is simple；Utilize magnetic agitation to make reaction more full and uniform, prepare the Sm with better photocatalytic activity2Sn2O7/SnO2Nano-complex, purity is high, and crystallinity is strong, and pattern is uniform.
[accompanying drawing explanation]
Fig. 1 is Sm prepared by the present invention2Sn2O7/SnO2The XRD figure of nano-complex；
Fig. 2 is Sm prepared by the present invention2Sn2O7/SnO2The photocatalysis performance figure of nano-complex.
[detailed description of the invention]
Embodiment 1:
1) by analytical pure SmCl3·6H2O and SnCl4·5H2O is dissolved in 10ml ethanol with the mol ratio of 1:0.1 and prepares Sm3+Concentration is the solution A of 0.022mol/L；
2) adopt analytical pure ammonia to regulate the pH to 7 of solution A, continue stirring 1h and form reaction precursor liquid；
3) being poured into by reaction precursor liquid in the hot inner bag of politef, heated sealed, react 10h at 100 DEG C, reaction naturally cools to room temperature after terminating；
4) product is successively with distilled water and dehydrated alcohol centrifuge washing 4 times, collects product vacuum drying 0.5h at 60 DEG C, obtains Sm2Sn2O7Product；
5) by analytical pure SnCl4·5H2The Sm of the 0.0242mol/L of O and 40ml2Sn2O7The mixed solution that solution is mixed to form puts into reactor, puts in baking oven after envelope still, reacts 3h at 100 DEG C, and reaction naturally cools to room temperature after terminating.Added SnCl4·5H2It is 2% that O accounts for the mass fraction of mixed solution.
6) product is successively with distilled water and dehydrated alcohol centrifuge washing 4 times, collects product vacuum drying 0.5h at 60 DEG C, obtains Sm2Sn2O7/SnO2Nano-complex.
Embodiment 2:
1) by analytical pure SmCl3·6H2O and SnCl4·5H2O is dissolved in 10ml ethanol with the mol ratio of 1:0.4 and prepares Sm3+Concentration is the solution A of 0.025mol/L；
2) adopt analytical pure ammonia to regulate the pH to 9 of solution A, continue stirring 1h and form reaction precursor liquid；
3) being poured into by reaction precursor liquid in the hot inner bag of politef, heated sealed, react 20h at 120 DEG C, reaction naturally cools to room temperature after terminating；
4) product is successively with distilled water and dehydrated alcohol centrifuge washing 4 times, collects product vacuum drying 0.7h at 65 DEG C, obtains Sm2Sn2O7Product；
5) by analytical pure SnCl4·5H2The mixed solution Sm that the solution of the 0.034mol/L of O and 40mol is mixed to form2Sn2O7Putting into reactor, put in baking oven after envelope still, react 3.5h at 120 DEG C, reaction naturally cools to room temperature after terminating；Added SnCl4·5H2It is 3% that O accounts for the mass fraction of mixed solution.
6) product is successively with distilled water and dehydrated alcohol centrifuge washing 4 times, collects product vacuum drying 0.7h at 60～80 DEG C, obtains Sm2Sn2O7/SnO2Nano-complex.
Embodiment 3:
1) by analytical pure SmCl3·6H2O and SnCl4·5H2O is dissolved in 10ml ethanol with the mol ratio of 1:0.6 and prepares Sm3+Concentration is the solution A of 0.05mol/L；
2) adopt analytical pure ammonia to regulate the pH to 10 of solution A, continue stirring 1.5h and form reaction precursor liquid；
3) being poured into by reaction precursor liquid in the hot inner bag of politef, heated sealed, react 25h at 140 DEG C, reaction naturally cools to room temperature after terminating；
4) product is successively with distilled water and dehydrated alcohol centrifuge washing 5 times, collects product vacuum drying 0.8h at 70 DEG C, obtains Sm2Sn2O7Product；
5) by analytical pure SnCl4·5H2The Sm of the 0.08mol/L of O and 40ml2Sn2O7The mixed solution that solution is mixed to form puts into reactor, puts in baking oven after envelope still, reacts 4h at 160 DEG C, and reaction naturally cools to room temperature after terminating.Added SnCl4·5H2It is 3.5% that O accounts for the mass fraction of mixed solution.
6) product is successively with distilled water and dehydrated alcohol centrifuge washing 5 times, collects product vacuum drying 0.8h at 70 DEG C, obtains Sm2Sn2O7/SnO2Nano-complex.
Embodiment 4:
1) by analytical pure SmCl3·6H2O and SnCl4·5H2O is dissolved in 10ml ethanol with the mol ratio of 1:0.8 and prepares Sm3+Concentration is the solution A of 0.08mol/L；
2) adopt analytical pure ammonia to regulate the pH to 11 of solution A, continue stirring 1.5h and form reaction precursor liquid；
3) being poured into by reaction precursor liquid in the hot inner bag of politef, heated sealed, react 35h at 180 DEG C, reaction naturally cools to room temperature after terminating；
4) product is successively with distilled water and dehydrated alcohol centrifuge washing 5 times, collects product vacuum drying 1.5h at 75 DEG C, obtains Sm2Sn2O7Product；
5) by analytical pure SnCl4·5H2The Sm of the 0.144mol/L of O and 40ml2Sn2O7The mixed solution that solution is mixed to form puts into reactor, puts in baking oven after envelope still, reacts 4.5h at 180 DEG C, and reaction naturally cools to room temperature after terminating.Added SnCl4·5H2It is 4.5% that O accounts for the mass fraction of mixed solution；
6) product is successively with distilled water and dehydrated alcohol centrifuge washing 5 times, collects product vacuum drying 1.5h at 75 DEG C, obtains Sm2Sn2O7/SnO2Nano-complex.
Embodiment 5:
1) by analytical pure SmCl3·6H2O and SnCl4·5H2O is dissolved in 10ml ethanol with the mol ratio of 1:1 and prepares Sm3+Concentration is the solution A of 0.08mol/L；
2) adopt analytical pure ammonia to regulate the pH to 13 of solution A, continue stirring 2h and form reaction precursor liquid；
3) being poured into by reaction precursor liquid in the hot inner bag of politef, heated sealed, react 0h at 200 DEG C, reaction naturally cools to room temperature after terminating；
4) product is successively with distilled water and dehydrated alcohol centrifuge washing 6 times, collects product vacuum drying 2h at 80 DEG C, obtains Sm2Sn2O7Product；
5) by analytical pure SnCl4·5H2The Sm of the 0.1001mol/L of O and 40ml2Sn2O7The mixed solution that solution is mixed to form puts into reactor, puts in baking oven after envelope still, reacts 5h at 200 DEG C, and reaction naturally cools to room temperature after terminating.Added SnCl4·5H2It is 5% that O accounts for the mass fraction of mixed solution.
6) product is successively with distilled water and dehydrated alcohol centrifuge washing 6 times, collects product vacuum drying 2h at 80 DEG C, obtains Sm2Sn2O7/SnO2Nano-complex.
Fig. 1 is Sm prepared by the present invention2Sn2O7/SnO2The XRD figure of nano-complex, as can be seen from the figure the purity of product is high, and crystallinity is strong.
Fig. 2 is Sm prepared by the present invention2Sn2O7/SnO2The photocatalysis performance figure of nano-complex, as can be seen from the figure prepared Sm2Sn2O7/SnO2The photocatalysis performance of nano-complex is compared with the Sm of single-phase2Sn2O7Nanometer product property has a distinct increment.
Claims (4)
1. tin dope solvent thermal-hydro-thermal method prepares Sm2Sn2O7/SnO2The method of nano-complex, it is characterised in that comprise the following steps:
1) by analytical pure SmCl3·6H2O and SnCl4·5H2O is with 1:(0.1～1) mol ratio be dissolved in organic solvent prepare Sm3+Concentration is the solution A of 0.022～0.08mol/L；
2) regulate the pH to 7～13 of solution A, continue stirring 1～2h and form reaction precursor liquid；
3) being poured into by reaction precursor liquid in the hot inner bag of politef, heated sealed, react 10～40h at 100～200 DEG C, reaction naturally cools to room temperature after terminating；
4) product washs, dries, and obtains Sm2Sn2O7；
5) by analytical pure SnCl4·5H2The Sm of O and 0.0242～0.144mol/L2Sn2O7The mixed solution that solution is mixed to form puts into reactor, puts in baking oven after envelope still, reacts 3～5h at 100～200 DEG C, and reaction naturally cools to room temperature after terminating；Added SnCl4·5H2It is 2%～5% that O accounts for the mass fraction of mixed solution；
6) product washs, dries, and obtains Sm2Sn2O7/SnO2Nano-complex；
Described organic solvent is ethanol.
2. a kind of tin dope solvent thermal-hydro-thermal method according to claim 1 prepares Sm2Sn2O7/SnO2The method of nano-complex is characterized in that: step 2) middle employing analytical pure ammonia adjustment pH value.
3. a kind of tin dope solvent thermal-hydro-thermal method according to claim 1 prepares Sm2Sn2O7/SnO2The method of nano-complex is characterized in that: step 4) described washing, dry particularly as follows: successively with distilled water and dehydrated alcohol centrifuge washing 4～6 times, collect product vacuum drying 0.5～2h at 60～80 DEG C.
4. a kind of tin dope solvent thermal-hydro-thermal method according to claim 1 prepares Sm2Sn2O7/SnO2The method of nano-complex is characterized in that: step 6) described washing, dry particularly as follows: successively with distilled water and dehydrated alcohol centrifuge washing 4～6 times, collect product vacuum drying 0.5～2h at 60～80 DEG C.
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