CN104549215B - Method for preparing Sm2O3/SnO2 nano composite by water bath process - Google Patents
Method for preparing Sm2O3/SnO2 nano composite by water bath process Download PDFInfo
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- CN104549215B CN104549215B CN201510026330.2A CN201510026330A CN104549215B CN 104549215 B CN104549215 B CN 104549215B CN 201510026330 A CN201510026330 A CN 201510026330A CN 104549215 B CN104549215 B CN 104549215B
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Abstract
The invention discloses a method for preparing a Sm2O3/SnO2 nano composite by a water bath process, which comprises the following steps: dissolving analytically pure SmCl3.6H2O in deionized water to obtain a solution A, dissolving analytically pure SnCl4.5H2O in distilled water to obtain a solution B, and magnetically stirring for completely dissolving; quickly adding the solution B into the solution A under the action of magnetic stirring to obtain a solution C; putting the solution C in a thermostatic water bath tank, reacting at 80-100 DEG C for 1-5 hours, and after the reaction finishes, naturally cooling to room temperature; and carrying out centrifuge washing on the product sequentially with distilled water and anhydrous ethanol 4-6 times, and drying in a 40-70-DEG C electrothermal vacuum drying oven for 1-5 hours, thereby obtaining the Sm2O3/SnO2 nano composite. The method has the advantages of accessible raw materials, low cost, simple technological equipment and low energy consumption; and by carrying out reaction under ordinary pressure and using water as the reaction solvent, the method also has the advantages of high safety and high feasibility.
Description
【Technical field】
The present invention relates to Nano semiconductor field of composite material preparation, and in particular to one kind prepares Sm2O3/SnO2Nanometer is multiple
The method of compound.
【Background technology】
Sm2O3It is a kind of broad stopband metal oxide with 4f electronic structures, energy gap is 4-6eV under normal temperature,
Sm2O3Crystal has three kinds of crystal formations, and when temperature is higher than 850 DEG C, monocline crystal transition is cube crystalline phase, in 2000 DEG C of left/right rotations
It is changed into hexagonal crystal phase, belongs to the oxide of polycrystalline inversion of phases, Sm2O3With high resistivity, high dielectric constant, high chemistry
The performance such as stability and heat endurance, with superior electricity, optics and magnetic performance, is widely used in ceramic capacitor, vapour
The aspects such as tailstock gas disposal, catalyst and medical science；In addition, nanometer Sm2O3Also there is nulcear properties, can be used as atomic reactor
The fields such as structural material, shielding material and control material.
SnO2With two kinds of crystal structures of tetragonal crystal system (rutile structure) and rhombic system, wherein orthorhombic phase is extremely unstable
It is fixed, can only exist under the high temperature conditions, SnO under normal circumstances2Crystal is all belonging to rutile structure.Pure SnO2Crystal is colourless
It is transparent, it is a kind of n-type semiconductor of important broad-band gap.Energy gap is 3.65eV, due to Sn electron affinity compared with
It is little, SnO2There is more Lacking oxygen in crystal, thus with N-type semiconductor characteristic.Nano SnO2With quantum size effect,
Thus can have broader energy gap, Senthilkumar et al. to prove nano SnO2Particle size is less, energy gap
Bigger, highest may be up to 4.26eV.
【The content of the invention】
It is an object of the invention to provide a kind of prepare Sm using immersion method2O3/SnO2The method of nano-complex, the party
The reaction medium of method is the aqueous solution, and safe, reaction raw materials are easy to get, and feasibility is strong, and process equipment is simple, using microwave hydrothermal
Make reaction more full and uniform, without the need for expensive reactor, do not limited by reaction volume volume, there is products therefrom preferable light to urge
Change activity.
To reach above-mentioned purpose, the technical solution used in the present invention is：
One kind prepares Sm using immersion method2O3/SnO2The method of nano-complex, comprises the following steps：
1) pure SmCl will be analyzed3·6H2O is dissolved in solvent the solution A for being obtained that molar concentration is 0.125～0.5mol/L；
2) pure SnCl will be analyzed4·5H2O is dissolved in distilled water the solution B for being obtained that molar concentration is 0.15～1mol/L, magnetic
Power is stirred to being completely dissolved；
3) solution B is rapidly added obtained solution C in solution A under magnetic agitation effect；Step 1) middle addition
SmCl3·6H2O and step 2) the middle SnCl for adding4·5H2The mol ratio of O is 1:(1～5)；
4) solution C is placed in constant water bath box, 1～5h is reacted at 80～100 DEG C, reaction naturally cools to room after terminating
Temperature；
5) after product washing, drying, Sm is obtained final product2O3/SnO2Nano-complex.
The solvent is deionized water.
The washing is specially：Successively with distilled water and absolute ethyl alcohol centrifuge washing 4～6 times.
The drying is specially：Product after washing is placed in 40～70 DEG C of electric vacunm drying casees and is dried 1～5h.Relatively
In prior art, the invention has the advantages that：
The present invention prepares Sm with immersion method2O3/SnO2Nano-complex, solution is placed in constant water bath box and is reacted, natural
It is cooled to product after room temperature, successively with distilled water and absolute ethyl alcohol centrifuge washing, to be placed in electric vacunm drying case and be dried 1～5h,
Obtain final product Sm (OH)3/SnO2Nano-complex, the Sm of gained2O3/SnO2Nano-complex purity is high, and crystallinity is strong, pattern it is uniform and
Good dispersion.The raw material of the reaction is easy to get and low cost, and process equipment is simple, and energy consumption is low, and the reaction is carried out at ambient pressure,
With water as reaction dissolvent, security is good, and feasibility is strong, so very economical, practicality, with good industrial prospect.
【Specific embodiment】
Embodiment 1：
1) 0.005mol is analyzed into pure SmCl3·6H2O is dissolved in 10ml deionized waters and molar concentration is obtained for 0.5mol/L
Solution A；
2) 0.005mol is analyzed into pure SnCl4·5H2O is dissolved in 10ml distilled water and molar concentration is obtained for 0.5mol/L's
Solution B, magnetic agitation is to being completely dissolved；
3) taken solution B is rapidly added obtained solution C in solution A under magnetic agitation effect；Step 1) middle addition
SmCl3·6H2O and step 2) the middle SnCl for adding4·5H2The mol ratio of O is 1:1；
4) solution C is placed in constant water bath box, 1h is reacted at 80 DEG C, reaction naturally cools to room temperature after terminating；
5) product is placed in 40 DEG C of electric vacunm drying casees and is dried successively with distilled water and absolute ethyl alcohol centrifuge washing 4 times
1h, obtains final product Sm2O3/SnO2Nano-complex.
Embodiment 2：
1) 0.005mol is analyzed into pure SmCl3·6H2O is dissolved in 20ml deionized waters and molar concentration is obtained for 0.25mol/L
Solution A；
2) 0.01mol is analyzed into pure SnCl4·5H2O is dissolved in 10ml distilled water and solution of the molar concentration for 1mol/L is obtained
B, magnetic agitation is to being completely dissolved；
3) taken solution B is rapidly added obtained solution C in solution A under magnetic agitation effect；Step 1) middle addition
SmCl3·6H2O and step 2) the middle SnCl for adding4·5H2The mol ratio of O is 1:2；
4) solution C is placed in constant water bath box, 2h is reacted at 90 DEG C, reaction naturally cools to room temperature after terminating；
5) product is placed in 50 DEG C of electric vacunm drying casees and is dried successively with distilled water and absolute ethyl alcohol centrifuge washing 5 times
2h, obtains final product Sm2O3/SnO2Nano-complex.
Embodiment 3：
1) 0.005mol is analyzed into pure SmCl3·6H2O is dissolved in 25ml deionized waters and molar concentration is obtained for 0.2mol/L
Solution A；
2) 0.015mol is analyzed into pure SnCl4·5H2O is dissolved in 10ml distilled water and molar concentration is obtained for 0.15mol/L's
Solution B, magnetic agitation is to being completely dissolved；Step 1) the middle SmCl for adding3·6H2O and step 2) the middle SnCl for adding4·5H2O
Mol ratio be 1：3；
3) taken solution B is rapidly added obtained solution C in solution A under magnetic agitation effect；
4) solution C is placed in constant water bath box, 3h is reacted at 95 DEG C, reaction naturally cools to room temperature after terminating；
5) product is placed in 55 DEG C of electric vacunm drying casees and is dried successively with distilled water and absolute ethyl alcohol centrifuge washing 5 times
3h, obtains final product Sm2O3/SnO2Nano-complex.
Embodiment 4：
1) 0.005mol is analyzed into pure SmCl3·6H2O is dissolved in 40ml deionized waters and molar concentration is obtained for 0.125mol/
The solution A of L；
2) 0.02mol is analyzed into pure SnCl4·5H2O is dissolved in 40ml distilled water and molar concentration is obtained for the molten of 0.5mol/L
Liquid B, magnetic agitation is to being completely dissolved；
3) taken solution B is rapidly added obtained solution C in solution A under magnetic agitation effect；Step 1) middle addition
SmCl3·6H2O and step 2) the middle SnCl for adding4·5H2The mol ratio of O is 1:4；
4) solution C is placed in constant water bath box, 4h is reacted at 100 DEG C, reaction naturally cools to room temperature after terminating；
5) product is placed in 60 DEG C of electric vacunm drying casees and is dried successively with distilled water and absolute ethyl alcohol centrifuge washing 5 times
4h, obtains final product Sm2O3/SnO2Nano-complex.
Embodiment 5：
1) 0.005mol is analyzed into pure SmCl3·6H2O is dissolved in 40ml deionized waters and molar concentration is obtained for 0.125mol/
The solution A of L；
2) 0.025mol is analyzed into pure SnCl4·5H2O is dissolved in 25ml distilled water and molar concentration is obtained for the molten of 1mol/L
Liquid B, magnetic agitation is to being completely dissolved；
3) taken solution B is rapidly added obtained solution C in solution A under magnetic agitation effect；Step 1) middle addition
SmCl3·6H2O and step 2) the middle SnCl for adding4·5H2The mol ratio of O is 1:5；
4) solution C is placed in constant water bath box, 5h is reacted at 100 DEG C, reaction naturally cools to room temperature after terminating；
5) product is placed in 70 DEG C of electric vacunm drying casees and is dried successively with distilled water and absolute ethyl alcohol centrifuge washing 6 times
5h, obtains final product Sm2O3/SnO2Nano-complex.
Sm2O3/SnO2Nano-complex is demonstrated by good photocatalysis performance in photocatalytic degradation methylene blue, ultraviolet
After irradiation 30min, reached 78.2% to organic matter degradation (and individually Sm2O3For 14.2%, single SnO2For
53.7%).
Claims (1)
1. it is a kind of that Sm is prepared using immersion method2O3/SnO2The method of nano-complex, it is characterised in that comprise the following steps：
1) pure SmCl will be analyzed3·6H2O is dissolved in solvent and solution A of the molar concentration for 0.5mol/L is obtained；
2) pure SnCl will be analyzed4·5H2O is dissolved in distilled water and solution B of the molar concentration for 0.5mol/L is obtained, and magnetic agitation is extremely
It is completely dissolved；
3) solution B is rapidly added obtained solution C in solution A under magnetic agitation effect；Step 1) the middle SmCl for adding3·
6H2O and step 2) the middle SnCl for adding4·5H2The mol ratio of O is 1:1；
4) solution C is placed in constant water bath box, 1h is reacted at 80 DEG C, reaction naturally cools to room temperature after terminating；
5) product is placed in 40 DEG C of electric vacunm drying casees and is dried 1h, i.e., successively with distilled water and absolute ethyl alcohol centrifuge washing 4 times
Obtain Sm2O3/SnO2Nano-complex；
The solvent is deionized water；
Sm2O3/SnO2Nano-complex after ultraviolet irradiation 30min, reaches in photocatalytic degradation methylene blue to organic matter degradation
To 78.2%.
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