CN107686131B - A kind of Sm2(MoO4)3The direct preparation method of film - Google Patents
A kind of Sm2(MoO4)3The direct preparation method of film Download PDFInfo
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- CN107686131B CN107686131B CN201710606776.1A CN201710606776A CN107686131B CN 107686131 B CN107686131 B CN 107686131B CN 201710606776 A CN201710606776 A CN 201710606776A CN 107686131 B CN107686131 B CN 107686131B
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a kind of Sm2(MoO4)3The direct preparation method of film.By Sm (NO3)3·6H2O is dissolved in the solution for being configured to that rare earth ion total concentration is 0.005 ~ 1mol/L in deionized water, and EDTA or citric acid, NaOH solution, Na are added wherein2MoO4·2H2O, KCl and HNO3, electric depositing solution is obtained after mixing, is placed in water-bath, its temperature is made to reach required temperature;Three-electrode system is inserted into electric depositing solution, thin film is being deposited on electro-conductive glass by electrodeposit reaction, film is being used respectively deionized water, dehydrated alcohol rinse, and is being subsequently placed in air dry oven dry, dried electrodeposited film is placed in tube furnace again to be heat-treated, Sm is made2(MoO4)3Film.Operation of the present invention is simple, compared to the conventional method to form a film after powder is first done, greatly simplifies method for manufacturing thin film, while avoiding influence of the powder morphology to quality of forming film;And method provided by the invention is easy to operate, and time-consuming short, film quality is good.
Description
Technical field
The invention belongs to materialogy technical fields, and in particular to a kind of Sm2(MoO4)3The direct preparation method of film.
Background technique
The rare earth luminescent material of molybdic acid salt system is because it is with good chemical stability and higher fluorescence quantum efficiency
The advantages that by the fluorescent material as fields such as solid state lighting, FPD, lasers, and fluorescent material is prepared into accordingly
Film is an important premise of luminescent material device.There are many rare earth molybdic acids that method can prepare different-shape at present
Salt material, such as sol-gel method, hydro-thermal method, solid phase method, microwave method etc..The principle of sol-gal process is alkoxide or esters
It closes object dissolution in organic solvent, by hydrolysis, forms activated monomer, monomer polymerize in turn forms colloidal sol, enables colloidal sol poly-
The gel for being formed and there is certain space structure is closed, drying and heat treatment remove organic matter therein, and sintering curing is formed
The nano material of required nano material, the molybdic acid salt system of this method preparation is mostly the inhomogenous nanometer rods in surface, and is easy
Reunite, the material of such pattern is not suitable for being made into film;Hydro-thermal method is to create the environment of a high temperature and pressure, keeps those big
Insoluble or indissoluble substance dissolution under the conditions of gas, or reaction generate the lysate of the substance, by molten in control autoclave
The temperature difference of liquid makes reactant generation convection current that growth crystal be precipitated to form hypersaturated state, the molybdic acid salt system of this method preparation
Nano material more be rendered as flower shape, each flower is made of multiple nanometer sheets, and these nanometer sheets are sufficiently stable, no
Easily dispersion, thus such pattern is also not suitable for being made into film;Solid phase method refers generally to participate in using solid matter and by the variation of phase
Manufacture a kind of method of powder, the powder granularity that this method is prepared is not thin enough, and inhomogenous, thus can not be prepared
The ideal pattern of high-quality thin film;Heating speed is fast, reaction rate is big, heating is equal because its technical characterstic has for microwave process for synthesizing
Even, product purity is high and reactant can selectively adjust the synthesis that the advantages that heating is widely used in nano material
Cheng Zhong, but the pattern of the product of microwave method preparation is easy to appear agglomeration, therefore the product obtained is not still to prepare height
The ideal chose of quality thin film.
To sum up, above method synthesis condition is relatively high, show that synthesis temperature is high and the requirement to reaction vessel also compared with
High two aspects;In addition to microwave method, the synthesis process of other methods is taken a long time;Most importantly received using obtained by the above method
The pattern of rice material is not suitable for preparing high quality light-emitting film, this makes its application receive great limitation.
Sm2(MoO4)3With good chemical stability, the present invention is being coated with conduction using three-electrode electro Chemical sedimentation
The film directly preparing respective films on the glass substrate of film, and preparing has a special microscopic appearance, easily and other materials
Carry out compound, this is of great significance for the device of material.
Summary of the invention
In view of the above-mentioned problems of the prior art, the object of the present invention is to provide a kind of Sm2(MoO4)3Film it is direct
Preparation method, this method directly obtain thin film using three-electrode electro Chemical deposition technique on the glass for be coated with conductive layer,
Process is simple, time-consuming shorter, and gained film is smooth and fine and close.
Specific steps are as follows:
(1) by Sm (NO3)3·6H2It is 0.005 ~ 1mol/L that O, which is dissolved in deionized water and is configured to rare earth ion total concentration,
Rare-earth ion solution, then EDTA or citric acid are added according to ratio that the molar ratio of rare earth ion total amount is 1 ~ 5:1
Enter into above-mentioned rare-earth ion solution, then the NaOH solution of 0.1 ~ 1mol/L be added dropwise until the pH value of mixed solution reaches 12 ~ 13,
Finally add Na2MoO4·2H2O, KCl and HNO3, wherein Na2MoO4·2H2The additional amount of O and mole of rare earth ion total amount
Than for 1 ~ 5:1, the additional amount of KCl and the molar ratio of rare earth ion total amount are 1 ~ 50:1, HNO3Additional amount for adjust mixing
The pH value of solution is 4 ~ 6, obtains electric depositing solution after mixing.
(2) electric depositing solution made from step (1) is placed in water-bath, stirring make the temperature of electric depositing solution reach 30 ~
80 DEG C, obtain spare electric depositing solution.
(3) glass of transparency conducting layer is coated with using surface as working electrode i.e. anode, Pt net is used as to electrode, that is, cathode,
Ag/AgCl/Cl-Electrode forms three-electrode system as reference electrode.
(4) in the spare electric depositing solution for obtaining the three-electrode system inserting step (2) of step (3) composition, setting is heavy
Product voltage is 1.3 ~ 3V, and sedimentation time is 15min ~ 3h, deposits one layer of electrodeposited film over transparent conductive layer.
(5) it uses deionized water, dehydrated alcohol to rinse respectively electrodeposited film made from step (4), is subsequently placed in 30 ~ 80
DEG C air dry oven in dry 5min ~ for 24 hours.
(6) the dried electrodeposited film of step (5) is placed in tube furnace and is heat-treated, setting heating rate be 1 ~
10 DEG C/min, 300 ~ 700 DEG C of 0.5 ~ 10h of heat preservation are warming up to, Sm is obtained2(MoO4)3Film.
The transparency conducting layer is ITO, FTO or AZO.
Compared with prior art, the features of the present invention and beneficial effect are:
Operation of the present invention is simple, is directly prepared on the glass substrate for be coated with conductive layer using electrochemical deposition method
Sm2(MoO4)3Film greatly simplifies method for manufacturing thin film, avoids simultaneously compared to the conventional method to form a film after powder is first done
Influence of the powder morphology to quality of forming film;And method provided by the invention is easy to operate, and time-consuming short, film quality is good.
Detailed description of the invention
Fig. 1 is the Sm of preparation of the embodiment of the present invention2(MoO4)3The XRD spectrum of film.
Fig. 2 is the Sm of preparation of the embodiment of the present invention2(MoO4)3The pictorial diagram of film.
Fig. 3 is the Sm of preparation of the embodiment of the present invention2(MoO4)3The SEM spectrum of film.
Specific embodiment
Embodiment:
Nitrate compound, citric acid, NaOH, the Na for the samarium (Sm) that the present embodiment uses2MoO4·2H2O、KCl、HNO3 ?
For commercially available analysis pure chemistry reagent.
Specific preparation process is as follows:
(1) by Sm (NO3)3·6H2O is dissolved in the rare earth for being configured to that rare earth ion concentration is 0.03mol/L in deionized water
Then citric acid is added to above-mentioned rare earth ion according to the molar ratio of rare earth ion total amount for the ratio of 3:1 by solion
In solution, then the NaOH solution of 1mol/L is added dropwise until the pH value of mixed solution reaches 12.7, finally adds Na2MoO4·
2H2O, KCl and HNO3, wherein Na2MoO4·2H2The molar ratio of the additional amount of O and rare earth ion total amount be 2:1, KCl and rare earth from
The molar ratio of sub- total amount is 35:1, HNO3Additional amount to be used to adjust the pH value of mixed solution be 5, it is heavy to obtain electricity after mixing
Product solution.
(2) electric depositing solution made from step (1) is placed in water-bath, stirring makes the temperature of electric depositing solution reach 80
DEG C, obtain spare electric depositing solution.
(3) glass of transparency conducting layer ITO is coated with using surface as working electrode i.e. anode, it is yin that Pt net, which is used as to electrode,
Pole, Ag/AgCl/Cl-Electrode forms three-electrode system as reference electrode.
(4) in the spare electric depositing solution for obtaining the three-electrode system inserting step (2) of step (3) composition, setting is heavy
Product voltage is 1.98V, sedimentation time 1h, deposits one layer of electrodeposited film over transparent conductive layer.
(5) it uses deionized water, dehydrated alcohol to rinse respectively electrodeposited film made from step (4), is subsequently placed in 40 DEG C
Air dry oven in dry 5min.
(6) the dried electrodeposited film of step (5) is placed in tube furnace and is heat-treated, setting heating rate is 10
DEG C/min, 500 DEG C of heat preservation 2h are warming up to, Sm is obtained2(MoO4)3Film.
Sm made from the embodiment of the present invention2(MoO4)3Film carries out XRD material phase analysis using X-ray diffractometer, using field
Emit scanning electron microscope and carry out morphology observation and analysis, is specifically shown in Figure of description 1,2 and 3.
Claims (1)
1. a kind of Sm2(MoO4)3The direct preparation method of film, it is characterised in that specific steps are as follows:
(1) by Sm (NO3)3·6H2O is dissolved in the rare earth for being configured to that rare earth ion concentration is 0.005 ~ 1mol/L in deionized water
Then ethylenediamine tetra-acetic acid (EDTA) or citric acid are 1 ~ 5:1 according to the molar ratio of rare earth ion total amount by solion
Ratio be added in above-mentioned rare-earth ion solution, then the NaOH solution of 0.1 ~ 1mol/L is added dropwise until the pH of mixed solution reaches
12.0 ~ 13.0, finally add Na2MoO4·2H2O, KCl and HNO3, wherein Na2MoO4·2H2The additional amount and rare earth ion of O
The molar ratio of total amount is 1 ~ 5:1, and the additional amount of KCl and the molar ratio of rare earth ion total amount are 1 ~ 50:1, HNO3Additional amount use
It is 4 ~ 6 in the pH value for adjusting mixed solution, obtains electric depositing solution after mixing;
(2) electric depositing solution made from step (1) being placed in water-bath, stirring makes the temperature of electric depositing solution reach 30 ~ 80 DEG C,
Obtain spare electric depositing solution;
(3) glass of transparency conducting layer is coated with using surface as working electrode i.e. anode, Pt net is used as to electrode, that is, cathode, Ag/
AgCl/Cl-Electrode forms three-electrode system as reference electrode;
(4) in the spare electric depositing solution for obtaining the three-electrode system inserting step (2) of step (3) composition, setting deposition electricity
Pressure is 1.98 ~ 3V, and sedimentation time is 15min ~ 3h, deposits one layer of electrodeposited film over transparent conductive layer;
(5) it uses deionized water, dehydrated alcohol to rinse respectively electrodeposited film made from step (4), is subsequently placed in 30 ~ 80 DEG C
Dry 5min in air dry oven ~ for 24 hours;
(6) the dried electrodeposited film of step (5) is placed in tube furnace and is heat-treated, setting heating rate is 1 ~ 10
DEG C/min, 300 ~ 700 DEG C of 0.5 ~ 10h of heat preservation are warming up to, Sm is obtained2(MoO4)3Film;
The transparency conducting layer is ITO, FTO or AZO.
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CN101962805B (en) * | 2010-10-15 | 2012-04-25 | 浙江大学 | Electrochemical preparation method of lanthanum phosphate or rare earth doped lanthanum phosphate film |
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Application publication date: 20180213 Assignee: Guangxi aid Energy Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000464 Denomination of invention: A Direct Preparation Method of Sm2(MoO4)3Films Granted publication date: 20190723 License type: Common License Record date: 20221228 |