CN107574466B - A kind of Pr2(MoO4)3The direct preparation method of film - Google Patents
A kind of Pr2(MoO4)3The direct preparation method of film Download PDFInfo
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- CN107574466B CN107574466B CN201710606799.2A CN201710606799A CN107574466B CN 107574466 B CN107574466 B CN 107574466B CN 201710606799 A CN201710606799 A CN 201710606799A CN 107574466 B CN107574466 B CN 107574466B
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- 229910015667 MoO4 Inorganic materials 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 20
- -1 rare earth ion Chemical class 0.000 claims abstract description 18
- 238000000151 deposition Methods 0.000 claims abstract description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011521 glass Substances 0.000 claims abstract description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 229910002828 Pr(NO3)3·6H2O Inorganic materials 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 21
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims description 6
- 239000011684 sodium molybdate Substances 0.000 claims description 6
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical group [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 34
- 238000000034 method Methods 0.000 abstract description 23
- 239000000843 powder Substances 0.000 abstract description 6
- 239000010409 thin film Substances 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000007796 conventional method Methods 0.000 abstract description 2
- 239000002659 electrodeposit Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229960001484 edetic acid Drugs 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical class O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000006166 lysate Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- Chemically Coating (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of Pr2(MoO4)3The direct preparation method of film.By Pr (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 used respectively deionized water, dehydrated alcohol rinse, it is subsequently placed in air dry oven dry, dried electrodeposited film is placed in again and is connected with the tube furnace of nitrogen and is heat-treated, Pr 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 Pr2(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.
Pr2(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 have special microscopic appearance, easily with other objects
Matter progress is 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 Pr2(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 Pr (NO3)3·6H2It is 0.005 ~ 1mol/L's that O, which is dissolved in and is configured to rare earth ion concentration in deionized water,
Then rare-earth ion solution EDTA or citric acid is added according to the molar ratio of rare earth ion total amount for the ratio of 1 ~ 5:1
Into above-mentioned rare-earth ion solution, then the NaOH solution of 0.1 ~ 1mol/L is added dropwise until the pH value of mixed solution reaches 12 ~ 13, most
After add Na2MoO4·2H2O, KCl and HNO3, wherein Na2MoO4·2H2The additional amount of O and the molar ratio of rare earth ion total amount
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 it is molten
The pH value of liquid 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 40 ~ 80
DEG C air dry oven in dry 5min ~ for 24 hours.
(6) the dried electrodeposited film of step (5) is placed in the tube furnace for be connected with nitrogen and is heat-treated, setting rises
Warm rate is 1 ~ 10 DEG C/min, is warming up to 300 ~ 700 DEG C of 0.5 ~ 10h of heat preservation, obtains Pr2(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
Pr2(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 Pr of preparation of the embodiment of the present invention2(MoO4)3The XRD spectrum of film.
Fig. 2 is the Pr of preparation of the embodiment of the present invention2(MoO4)3The pictorial diagram of film.
Fig. 3 is the Pr of preparation of the embodiment of the present invention2(MoO4)3The SEM spectrum of film.
Specific embodiment
Embodiment:
Nitrate compound, the ethylenediamine tetra-acetic acid (EDTA), NaOH, Na for the spectrum (Pr) that the present embodiment uses2MoO4·
2H2O、KCl、HNO3 It is commercially available analysis pure chemistry reagent.
Specific preparation process is as follows:
(1) by Pr (NO3)3·6H2It is the dilute of 0.2mol/L that O, which is dissolved in and is configured to rare earth ion total concentration in deionized water,
Then EDTA 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 native solion
In solution, then be added dropwise 0.5mol/L NaOH solution until mixed solution pH be 12.6, finally add Na2MoO4·2H2O、
KCl and HNO3, wherein Na2MoO4·2H2The additional amount of O and the molar ratio of rare earth ion total amount are 2:1, and KCl is total with rare earth ion
The molar ratio of amount is 25:1, HNO3Additional amount be used for adjust mixed solution pH value be 6, after mixing obtain electro-deposition it is molten
Liquid.
(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 2.0V, 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 the tube furnace for be connected with nitrogen and is heat-treated, setting rises
Warm rate is 3 DEG C/min, is warming up to 500 DEG C of heat preservation 1h, obtains Pr2(MoO4)3Film.
Pr 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 Pr2(MoO4)3The direct preparation method of film, it is characterised in that specific steps are as follows:
(1) by Pr (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 edta edta or citric acid are 1 ~ 5:1's according to the molar ratio of rare earth ion total amount by solion
Ratio is 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 2.0 ~ 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 40 ~ 80 DEG C
Dry 5min in air dry oven ~ for 24 hours；
(6) the dried electrodeposited film of step (5) is placed in the tube furnace for be connected with nitrogen and is heat-treated, setting heating speed
Rate is 1 ~ 10 DEG C/min, is warming up to 300 ~ 700 DEG C of 0.5 ~ 10h of heat preservation, obtains Pr2(MoO4)3Film；
The transparency conducting layer is ITO, FTO or AZO.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710606799.2A CN107574466B (en) | 2017-07-24 | 2017-07-24 | A kind of Pr2(MoO4)3The direct preparation method of film |
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| CN201710606799.2A CN107574466B (en) | 2017-07-24 | 2017-07-24 | A kind of Pr2(MoO4)3The direct preparation method of film |
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| CN107574466B true CN107574466B (en) | 2019-11-26 |
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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: 20180112 Assignee: Guilin Qiyun New Materials Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044281 Denomination of invention: A Direct Preparation Method for Pr2(MoO4)3Thin Films Granted publication date: 20191126 License type: Common License Record date: 20231026 |
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