CN104588025B - A kind of self assembly near-spherical Sm2o3the preparation method of/CuO nano-complex - Google Patents

A kind of self assembly near-spherical Sm2o3the preparation method of/CuO nano-complex Download PDF

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CN104588025B
CN104588025B CN201510026087.4A CN201510026087A CN104588025B CN 104588025 B CN104588025 B CN 104588025B CN 201510026087 A CN201510026087 A CN 201510026087A CN 104588025 B CN104588025 B CN 104588025B
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spherical
reaction
self assembly
complex
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CN104588025A (en
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殷立雄
韩鑫
裴宇梁
宋华虎
张东东
黄剑锋
孔新刚
柴思敏
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Shenzhen Huiyide Environmental Protection Material Co ltd
Zhejiang Hongsheng Technology Transfer Services Co ltd
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Shaanxi University of Science and Technology
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Abstract

Open a kind of self assembly near-spherical Sm of the present invention2O3The preparation method of/CuO nano-complex: by SmCl3·6H2O joins deionized water middle obtained solution A under magnetic stirring;By CuCl2·2H2O dissolves in deionized water under magnetic stirring and forms solution B;Than mixing and the pH to 5~8 of ammonia spirit regulation solution is used to form reaction precursor liquid according to different volumes two parts of solution of A, B;Pouring in water heating kettle by reaction precursor liquid, envelope still is rearmounted to enter to carry out hydro-thermal reaction in microwave hydrothermal reaction, and reaction naturally cools to room temperature after terminating;Sample is centrifuged washing and carries out drying and be placed in Muffle furnace at 500~800 DEG C calcining and 2~5h i.e. obtain self assembly near-spherical Sm2O3/ CuO nano-complex.The reaction medium of the inventive method is aqueous solution, and safety is high, and reaction raw materials is easy to get, and feasibility is strong, and process equipment is simple.

Description

A kind of self assembly near-spherical Sm2O3The preparation method of/CuO nano-complex
[technical field]
The invention belongs to Nano semiconductor field of composite material preparation, be specifically related to a kind of Sm2O3The preparation method of/CuO nano-complex.
[background technology]
Sm2O3It is a kind of pale yellow powder, easy deliquescence, water insoluble, it is soluble in energy converslon materials and optoelectronic thin film material, nano level Sm that mineral acid is a new generation2O3In multiple fields of the functional materials such as high efficiency light-emitting device, magnetic material, catalysis material, there is potential using value.As wide bandgap semiconductor, it has considerable research and application prospect in terms of photocatalysis degradation organic contaminant.
Sm2O3As a kind of wide bandgap semiconductor, in terms of light degradation Organic substance, there is preferable Research Prospects, but because of forbidden band wider (Eg=4.4eV), relatively low to the responsiveness of visible spectrum.
[summary of the invention]
It is an object of the invention to provide a kind of self assembly near-spherical Sm2O3The preparation method of/CuO nano-complex, the method is safe and efficient, application is strong, process equipment is simple, prepared self assembly near-spherical Sm2O3/ CuO nano-complex, purity is high, and crystallinity is strong, and pattern is uniform, has preferable photocatalytic activity.
For reaching above-mentioned purpose, the technical solution used in the present invention is:
A kind of self assembly near-spherical Sm2O3The preparation method of/CuO nano-complex, comprises the following steps:
1) first, by analytical pure SmCl3·6H2It is 0.5~2mol/L solution A that O is dissolved in solvent prepared concentration under magnetic stirring;By CuCl2·2H2O dissolves under magnetic stirring and forms the solution B that concentration is 0.5~2mol/L in solvent;
2) secondly, by two parts of solution of A, B according to 1:(0.5~2) volume ratio mix and regulate pH to the 5~8 formation reaction precursor liquid of mixed solution;
3) then, pouring in water heating kettle by reaction precursor liquid, compactedness is 55%~75%, puts in microwave hydrothermal reaction after envelope still, reacts 0.5~2h at 100~200 DEG C, and reaction naturally cools to room temperature after terminating;
4) last, product is washed, calcines, obtain self assembly near-spherical Sm2O3/ CuO nano-complex.
Step 1) in the solvent of solution A and solution B be deionized water.
Step 2) in use mass percent be 5%~10% ammonia spirit regulation mixed solution pH value.
Step 4) described in wash, calcine particularly as follows: successively with distilled water and dehydrated alcohol centrifuge washing 4~be placed on Muffle furnace for 6 times and calcine 2~5h at 500~800 DEG C.
The model of microwave hydrothermal reaction is MDS-10 type.
Relative to prior art, the method have the advantages that
React in the liquid phase due to the present invention and prepare self assembly near-spherical Sm through Technology for Heating Processing2O3The nano combined powder of/CuO, process equipment is simple, low cost, and manufacturing cycle is shorter, and Product size is uniform, good dispersion.
The present invention prepares a kind of self assembly near-spherical Sm2O3/ CuO nano-complex, reaction medium is aqueous solution, and safety is high, and reaction raw materials is easy to get, and feasibility is strong, and process equipment is simple.The stirring utilizing microwave can realize on molecular level as heating tool, has firing rate fast, homogeneous heating, without thermograde, without hysteresis effect, Product size is evenly distributed, good dispersion, and the product purity prepared through Technology for Heating Processing again after microwave hydrothermal is high, good crystallinity.
Sm2O3As a kind of wide bandgap semiconductor, in terms of light degradation Organic substance, there is preferable Research Prospects, but because of forbidden band wider (Eg=4.4eV), relatively low to the responsiveness of visible spectrum.But the recombination probability of its photo-generate electron-hole pair is greatly reduced, can carry out compound with the part that compensates its defect with low-gap semiconductor.As low-gap semiconductor, at the bottom of the conduction band of CuO, compare H+/H2Just, energy gap is 1.7eV to oxidation-reduction potential, and the response to visible spectrum is stronger.After both are combined by the present invention, CuO can effectively absorb visible ray as light-absorption layer so that photo-generate electron-hole is to efficiently separating, and protects CuO not by photoetch, thus improves photocatalysis efficiency.
[accompanying drawing explanation]
Fig. 1 is self assembly near-spherical Sm prepared by the present invention2O3The SEM figure of/CuO nano-complex.
[detailed description of the invention]
Embodiment 1:
1) first, by analytical pure SmCl3·6H2It is 0.5mol/L solution A that O is dissolved in appropriate amount of deionized water prepared concentration under magnetic stirring;By CuCl2·2H2It is the solution B of 0.5mol/L that O dissolve in deionized water under magnetic stirring to form concentration;
2) pH to 7 of the ammonia spirit regulation solution secondly, mixed according to the volume ratio of 1:1 by two parts of solution of A, B, heated and use mass percent to be 5% forms reaction precursor liquid;
3) then, pouring in water heating kettle by reaction precursor liquid, compactedness is 55%, puts in microwave hydrothermal reaction after envelope still, reacts 2h at 200 DEG C, and reaction naturally cools to room temperature after terminating;
4) last, with distilled water and dehydrated alcohol, sample centrifuge washing 4~6 times are placed on Muffle furnace successively at 600 DEG C, calcine 3h, obtain self assembly near-spherical Sm2O3/ CuO nano-complex.
Embodiment 2:
1) first, by analytical pure SmCl3·6H2It is 1mol/L solution A that O is dissolved in appropriate amount of deionized water prepared concentration under magnetic stirring;By CuCl2·2H2It is the solution B of 0.5mol/L that O dissolve in deionized water under magnetic stirring to form concentration;
2) pH to 5.5 of the ammonia spirit regulation solution secondly, mixed according to the volume ratio of 1:0.5 by two parts of solution of A, B, heated and use mass percent to be 8% forms reaction precursor liquid;
3) then, pouring in water heating kettle by reaction precursor liquid, compactedness is 60%, puts in microwave hydrothermal reaction after envelope still, reacts 2h at 150 DEG C, and reaction naturally cools to room temperature after terminating;
4) last, with distilled water and dehydrated alcohol, sample centrifuge washing 4~6 times are placed on Muffle furnace successively at 800 DEG C, calcine 2h, obtain self assembly near-spherical Sm2O3/ CuO nano-complex.
Embodiment 3:
1) first, by analytical pure SmCl3·6H2It is 2mol/L solution A that O is dissolved in appropriate amount of deionized water prepared concentration under magnetic stirring;By CuCl2·2H2It is the solution B of 1mol/L that O dissolve in deionized water under magnetic stirring to form concentration;
2) pH to 8 of the ammonia spirit regulation solution secondly, mixed according to the volume ratio of 1:2 by two parts of solution of A, B, heated and use mass percent to be 10% forms reaction precursor liquid;
3) then, pouring in water heating kettle by reaction precursor liquid, compactedness is 75%, puts in microwave hydrothermal reaction after envelope still, reacts 2h at 120 DEG C, and reaction naturally cools to room temperature after terminating;
4) last, with distilled water and dehydrated alcohol, sample centrifuge washing 4~6 times are placed on Muffle furnace successively at 600 DEG C, calcine 4h, obtain self assembly near-spherical Sm2O3/ CuO nano-complex.
Embodiment 4:
1) first, by analytical pure SmCl3·6H2It is 0.5mol/L solution A that O is dissolved in appropriate amount of deionized water prepared concentration under magnetic stirring;By CuCl2·2H2It is the solution B of 2mol/L that O dissolve in deionized water under magnetic stirring to form concentration;
2) pH to 5 of the ammonia spirit regulation solution secondly, mixed according to the volume ratio of 1:2 by two parts of solution of A, B, heated and use mass percent to be 5% forms reaction precursor liquid;
3) then, pouring in water heating kettle by reaction precursor liquid, compactedness is 75%, puts in microwave hydrothermal reaction after envelope still, reacts 1.5h at 150 DEG C, and reaction naturally cools to room temperature after terminating;
4) last, with distilled water and dehydrated alcohol, sample centrifuge washing 4~6 times are placed on Muffle furnace successively at 700 DEG C, calcine 2h, obtain self assembly near-spherical Sm2O3/ CuO nano-complex.
Embodiment 5:
1) first, by analytical pure SmCl3·6H2It is 0.5mol/L solution A that O is dissolved in appropriate amount of deionized water prepared concentration under magnetic stirring;By CuCl2·2H2It is the solution B of 1mol/L that O dissolve in deionized water under magnetic stirring to form concentration;
2) pH to 6 of the ammonia spirit regulation solution secondly, mixed according to the volume ratio of 1:1 by two parts of solution of A, B, heated and use mass percent to be 10% forms reaction precursor liquid;
3) then, pouring in water heating kettle by reaction precursor liquid, compactedness is 70%, puts in microwave hydrothermal reaction after envelope still, reacts 1h at 100 DEG C, and reaction naturally cools to room temperature after terminating;
4) last, with distilled water and dehydrated alcohol, sample centrifuge washing 4~6 times are placed on Muffle furnace successively at 800 DEG C, calcine 2h, obtain self assembly near-spherical Sm2O3/ CuO nano-complex.
Fig. 1 is self assembly near-spherical Sm prepared by the present invention2O3The SEM figure of/CuO nano-complex, the as can be seen from the figure good dispersion of product, in terms of photocatalytic degradation Organic substance, there is considerable application prospect.Sm2O3/ CuO nano-complex is demonstrated by good photocatalysis performance in photocatalytic degradation rhodamine B, after ultra-vioket radiation 30min, organic degraded has been reached 79.3% (and individually Sm2O3Being 11.3%, single CuO is 54.6%).

Claims (5)

1. self assembly near-spherical Sm2O3The preparation method of/CuO nano-complex, it is characterised in that bag Include following steps:
1) first, by analytical pure SmCl3·6H2It is 0.5~2 that O is dissolved in solvent prepared concentration under magnetic stirring Mol/L solution A;By CuCl2·2H2It is 0.5~2mol/L that O dissolves in formation concentration in solvent under magnetic stirring Solution B;
2) secondly, by two parts of solution of A, B according to 1:(0.5~2) volume ratio mix and regulate mixed solution PH to 5~8 formed reaction precursor liquid;
3) then, pouring in water heating kettle by reaction precursor liquid, compactedness is 55%~75%, puts into micro-after envelope still In ripple hydro-thermal reaction instrument, reacting 0.5~2h at 100~200 DEG C, reaction naturally cools to room temperature after terminating;
4) last, product is washed, calcines, obtain self assembly near-spherical Sm2O3/ CuO nano-complex.
A kind of self assembly near-spherical Sm the most according to claim 12O3The preparation of/CuO nano-complex Method, it is characterised in that: step 1) in the solvent of solution A and solution B be deionized water.
A kind of self assembly near-spherical Sm the most according to claim 12O3The preparation of/CuO nano-complex Method, it is characterised in that: step 2) the middle ammonia spirit regulation mixing using mass percent to be 5%~10% The pH value of solution.
A kind of self assembly near-spherical Sm the most according to claim 12O3The preparation of/CuO nano-complex Method, it is characterised in that: step 4) described in wash, calcine particularly as follows: successively by distilled water and anhydrous second Alcohol centrifuge washing 4~be placed on Muffle furnace for 6 times and calcine 2~5h at 500~800 DEG C.
A kind of self assembly near-spherical Sm the most according to claim 12O3The preparation of/CuO nano-complex Method, it is characterised in that: the model of microwave hydrothermal reaction is MDS-10 type.
CN201510026087.4A 2015-01-19 2015-01-19 A kind of self assembly near-spherical Sm2o3the preparation method of/CuO nano-complex Expired - Fee Related CN104588025B (en)

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CN104030335A (en) * 2014-06-20 2014-09-10 陕西科技大学 Method for preparing Sm(OH)3/ZnO nano-composite by using homogeneous hydrothermal method

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CN104030335A (en) * 2014-06-20 2014-09-10 陕西科技大学 Method for preparing Sm(OH)3/ZnO nano-composite by using homogeneous hydrothermal method

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