CN106544019A - A kind of morphology controllable NaGd (MoO4)2:Eu3+The preparation method of luminescent powder - Google Patents
A kind of morphology controllable NaGd (MoO4)2:Eu3+The preparation method of luminescent powder Download PDFInfo
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- CN106544019A CN106544019A CN201610830491.1A CN201610830491A CN106544019A CN 106544019 A CN106544019 A CN 106544019A CN 201610830491 A CN201610830491 A CN 201610830491A CN 106544019 A CN106544019 A CN 106544019A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7794—Vanadates; Chromates; Molybdates; Tungstates
Abstract
A kind of morphology controllable NaGd (MoO4) 2:The preparation method of Eu3+ luminescent powders, is related to a kind of rear-earth-doped luminous material preparation method, comprises the following steps：（1）Prepare the compound nitrate of rare earth（Gadolinium trinitrate and europium nitrate）Mixed solution；（2）Add sodium citrate and sodium molybdate（3）Mixed solution is carried out into hydro-thermal reaction under different sodium citrate ratios and pH value condition；（4）Washing, drying obtain product.The present invention is with Gd2O3 (99.99%), Eu2O3 (99.99%), analytically pure sodium molybdate（Na2MoO4•2H2O）, analytically pure sodium citrate (C6H5Na3O7 2H2O) prepares the NaGd (MoO4) 2 of different-shape for raw material using hydro-thermal method:Eu3+ luminescent powders, with easy to operate, reaction efficiency is high and the features such as strong process controllability；Synthesized NaGd (MoO4) 2:Eu3+ fluorescent material has morphology controllable, degree of crystallinity height, good dispersion, and has the advantages that good luminescent properties.
Description
Technical field
The present invention relates to a kind of rear-earth-doped luminous material preparation method, more particularly to a kind of morphology controllable NaGd
(MoO4)2:Eu3+The preparation method of luminescent powder.
Background technology
Bimetallic molybdate NaGd (MoO4) 2 due to its architectural characteristic and preferable physical and chemical stability, luminous, sharp
The Material Fields such as light, flicker and catalysis have potential application.Particularly molybdate has preferably absorption in ultra-violet (UV) band, and will can inhale
Receive energy and preferably pass to rare earth luminous ion, and as its construction features can also be such that spectrum widens and high-concentration dopant, this
A little features have caused the very big concern of people.As the important member in molybdic acid salt system, the common synthesis side of NaGd (MoO4) 2
Method is mainly solid-phase synthesis, hydro-thermal method and czochralski method.Wherein hydro-thermal method has that reaction temperature is gentle, synthetic method simple, brilliant
The features such as grain growth promoter is complete, granule is uniform, is applied to the synthesis of 2 fluorescent material of NaGd (MoO4).In the last few years, also in succession
The research of the regulation and control to 2 fluorescent material patterns of NaGd (MoO4) is carried out.For example：Anming Li et al. are by changing rare earth ion
The change procedure of 2 crystal of NaGd (MoO4) is observed with the mol ratio and regulation solution ph of sodium molybdate（Anming Li,
Dekang Xu, Hao Lin, Shenghong Yang, et al. Facile morphology-controllable
hydrothermal synthesis and color tunable luminescence properties of NaGd
(MoO4)2:Eu3+,Tb3+ microcrystals. RSC Adv., 2015;5:45693-45702）；Lanfen Li et al.
NaGd (MoO4) 2 has been synthesized using hydro-thermal method:Ln3+ (Ln=Eu, Tb, Dy, Sm) fluorescent material, have studied the photism of different ions
Can be with impact of the pH value to fluorescent material pattern and luminous intensity（Lanfen Li, Dongbing Dong, Jiying Zhang,
et al. Well-defined NaGd(MoO4)2:Ln3+(Ln=Eu,Tb,Dy,Sm) luminescent materials:
Facile synthesis and luminescence properties. Materials Letters, 2014;131:
298-301）.Existing research shows：The shape characteristic of luminescent powder has large effect for luminescent properties.Effective control molybdic acid
The research of gadolinium sodium nano material crystal morphology is significant.
Sodium citrate in inorganic nano material synthetic system, there is obvious structure to lead as a kind of typical chelating agent
To effect, the features such as which has good dissolubility, latent, complexing, surface activity and stable chemical nature, can be anti-
Effectively slow down the nucleation rate and complex rare-earth ion of crystal, and then the formation of Effective Regulation crystal in answering system, to inorganic
The pattern of nano material is effectively controlled.
The content of the invention
It is an object of the invention to provide a kind of morphology controllable NaGd (MoO4) 2:The preparation method of Eu3+ luminescent powders, the party
Method prepares NaGd (MoO4) 2 using hydro-thermal method with sodium citrate as chelating agent:Eu3+ luminescent powders.The method have it is easy to operate,
The features such as repetitive rate height and strong controllability；Synthesized NaGd (MoO4) 2:Eu3+ fluorescent material has morphology controllable, degree of crystallinity
The advantages of high, good dispersion.
The purpose of the present invention is achieved through the following technical solutions：
A kind of morphology controllable NaGd (MoO4) 2:The preparation method of Eu3+ luminescent powders, methods described with Gd2O3 (99.99%),
Eu2O3 (99.99%), analytically pure sodium molybdate（Na2MoO4•2H2O）With analytically pure sodium citrate（C6H5Na3O7•2H2O）
For raw material, from the hydro-thermal method synthetic technology of sodium citrate auxiliary；
Comprise the following steps that：
（1）Gd2O3 and Eu2O3 are used into 1:1 (V/V) nitric acid dissolves, and adds deionized water to be prepared into the compound nitrate mixing of rare earth
Solution；
（2）Add sodium citrate；
（3）Sodium molybdate is added, precursor solution is uniformly mixing to obtain；
（4）Adjust the pH value of presoma；
（5）The precursor solution adjusted after pH value is transferred in the reactor that liner is politef, hydro-thermal reaction is sealed
After kettle, react a few hours under the conditions of preset temperature, reaction naturally cools to room temperature after terminating, and obtains white precipitate；
（6）The white precipitate for generating is taken out, for several times, being dried a few hours under the conditions of preset temperature obtains NaGd (MoO4) for washing
2:Eu3+ luminescent powders.
A kind of described morphology controllable NaGd (MoO4) 2:The preparation method of Eu3+ luminescent powders, step（1）Middle Eu3+ is accounted for
（Gd3++ Eu3+）Mole percent ratio be 2.5-10%.
A kind of described morphology controllable NaGd (MoO4) 2:The preparation method of Eu3+ luminescent powder luminescent properties, step（2）In
It is 1 according to rare earth ion and sodium citrate mol ratio：0.5-2 adds sodium citrate.
A kind of described pattern that adjusts strengthens NaGd (MoO4) 2:The preparation method of Eu3+ luminescent powder luminescent properties, step
（3）In be 14 according to rare earth ion and sodium molybdate mol ratio:3 add sodium molybdate.
A kind of described morphology controllable NaGd (MoO4) 2:The preparation method of Eu3+ luminescent powder luminescent properties, step（4）In
HNO3 and NaOH is adopted to adjust pH value for 5-7.
A kind of described morphology controllable NaGd (MoO4) 2:The preparation method of Eu3+ luminescent powder luminescent properties, step（5）In advance
If reaction temperature is 170-190 DEG C, sufficient reaction time is 20-48h.
A kind of described morphology controllable NaGd (MoO4) 2:The preparation method of Eu3+ luminescent powder luminescent properties, step（6）It is dry
Dry temperature 60-80 DEG C, time are 12-24h.
Advantages of the present invention with effect is：
The present invention is synthesized with rare earth oxide as raw material using hydro-thermal method, by adjusting rare earth ion and sodium citrate mol ratio
Come to NaGd (MoO4) 2:The pattern of Eu3+ luminescent powders is regulated and controled, and the NaGd (MoO4) 2 of different morphologies has been obtained:Eu3+ is brilliant
Body, crystal morphology are regular, and crystallite dimension is homogeneous, and degree of crystallinity is high and good dispersion.Wherein obtained NaGd (MoO4) 2:Eu3+
Luminescent powder has good luminescent properties.With sodium citrate as surfactant, whole reaction is carried out the present invention in aqueous,
Economic and environment-friendly, process is simple, easy to operate and short preparation period, are with a wide range of applications.Provide simultaneously a kind of of the same race
Regulate and control the new method of pattern under crystal structure, one kind is provided to the impact for lighting for pattern under the conditions of research crystalline phase of the same race and is newly thought
Road.
Description of the drawings
Fig. 1 is NaGd (MoO4) 2 prepared by embodiment 3:The SEM figures of Eu3+ luminescent powders；
Fig. 2 is NaGd (MoO4) 2 prepared by example 5:The SEM figures of Eu3+ luminescent powders；
Fig. 3 is NaGd (MoO4) 2 prepared by embodiment 3 and example 5:The XRD spectra of Eu3+ luminescent powders；
Fig. 4 is NaGd (MoO4) 2 prepared by embodiment 3 and example 5:The launching light spectrogram of Eu3+ luminescent powders.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
Embodiment 1：The Eu (NO3) 3 for measuring the 29.25mlGd (NO3) 3 and 0.75ml of 0.1mol/L concentration respectively is dissolved in burning
In cup, mix；It is 1 according to rare earth ion and sodium citrate mol ratio:0.5 adds sodium citrate in mixed solution, treats
After sodium citrate dissolving, then continuing magnetic force stirring 30min under room temperature weighs 0.7945g sodium molybdate and adds above-mentioned mixed solution
After middle all dissolvings, it is 7 to adjust solution ph with HNO3 and NaOH, continues stirring 1h；Mixed solution is transferred to into liner for poly- four
In the 50mL reactors of fluorothene, the packing ratio of hydrothermal reaction kettle is 80%, seals hydrothermal reaction kettle；Hydrothermal reaction kettle is put into
In baking oven, 24h is incubated from room temperature to after 180 DEG C, then naturally cools to room temperature；Product in hydrothermal reaction kettle is centrifuged
Afterwards, deionized water and dehydrated alcohol are washed 2 times respectively, are dried 24h at 60 DEG C, you can obtain NaGd (MoO4) 2:Eu3+ length and width
Than close similar square particle light-emitting powder.
Embodiment 2：The Eu (NO3) 3 for measuring the 29.25mlGd (NO3) 3 and 0.75ml of 0.1mol/L concentration respectively is dissolved in burning
In cup, mix；It is 1 according to rare earth ion and sodium citrate mol ratio:1 adds sodium citrate in mixed solution, treats lemon
After lemon acid sodium dissolving, then continuing magnetic force stirring 30min under room temperature is weighed in the above-mentioned mixed solution of 0.7945g sodium molybdate addition
After all dissolving, it is 7 to adjust solution ph with HNO3 and NaOH, continues stirring 1h；Mixed solution is transferred to into liner for polytetrafluoro
In the 50mL reactors of ethylene, the packing ratio of hydrothermal reaction kettle is 80%, seals hydrothermal reaction kettle；Hydrothermal reaction kettle is put into into baking
In case, 36h is incubated from room temperature to after 180 DEG C, then naturally cools to room temperature；Product in hydrothermal reaction kettle is centrifuged
Afterwards, deionized water and dehydrated alcohol are washed 2 times respectively, are dried 24h at 60 DEG C, you can obtain NaGd (MoO4) 2:The little chis of Eu3+
Very little rice particle shape particle light-emitting powder.
Embodiment 3：The Eu (NO3) 3 for measuring the 27.0mlGd (NO3) 3 and 3.0ml of 0.1mol/L concentration respectively is dissolved in beaker
In, mix；It is 1 according to rare earth ion and sodium citrate mol ratio:1.5 adding citric acid sodium treat Fructus Citri Limoniae in mixed solution
After the dissolving of sour sodium, continuing magnetic force stirring 30min under room temperature, then weigh 0.7945g sodium molybdate add it is complete in above-mentioned mixed solution
After portion's dissolving, it is 7 to adjust solution ph with HNO3 and NaOH, continues stirring 1h；Mixed solution is transferred to into liner for polytetrafluoroethyl-ne
In the 50mL reactors of alkene, the packing ratio of hydrothermal reaction kettle is 80%, seals hydrothermal reaction kettle；Hydrothermal reaction kettle is put into into baking oven
In, 20h is incubated from room temperature to after 190 DEG C, then naturally cools to room temperature；After by product centrifugation in hydrothermal reaction kettle,
Deionized water and dehydrated alcohol are washed 2 times respectively, are dried 12h at 80 DEG C, you can obtain NaGd (MoO4) 2:The larger chis of Eu3+
Very little rice particle shape particle light-emitting powder.
Embodiment 4：The Eu (NO3) 3 for measuring the 28.5mlGd (NO3) 3 and 1.5ml of 0.1mol/L concentration respectively is dissolved in beaker
In, mix；It is 1 according to rare earth ion and sodium citrate mol ratio:2 add sodium citrate in mixed solution, treat Fructus Citri Limoniae
After the dissolving of sour sodium, continuing magnetic force stirring 30min under room temperature, then weigh 0.7945g sodium molybdate add it is complete in above-mentioned mixed solution
After portion's dissolving, it is 7 to adjust solution ph with HNO3 and NaOH, continues stirring 1h；Mixed solution is transferred to into liner for polytetrafluoroethyl-ne
In the 50mL reactors of alkene, the packing ratio of hydrothermal reaction kettle is 80%, seals hydrothermal reaction kettle；Hydrothermal reaction kettle is put into into baking oven
In, 48h is incubated from room temperature to after 170 DEG C, then naturally cools to room temperature；After by product centrifugation in hydrothermal reaction kettle,
Deionized water and dehydrated alcohol are washed 2 times respectively, are dried 18h at 70 DEG C, you can obtain NaGd (MoO4) 2:Eu3+ length-width ratios
Larger block particle light-emitting powder.
Embodiment 5：The Eu (NO3) 3 for measuring the 27.9mlGd (NO3) 3 and 2.1ml of 0.1mol/L concentration respectively is dissolved in beaker
In, mix；It is 1 according to rare earth ion and sodium citrate mol ratio:1 adds sodium citrate in mixed solution, treats Fructus Citri Limoniae
After the dissolving of sour sodium, continuing magnetic force stirring 30min under room temperature, then weigh 0.7945g sodium molybdate add it is complete in above-mentioned mixed solution
After portion's dissolving, it is 5 to adjust solution ph with HNO3 and NaOH, continues stirring 1h；Mixed solution is transferred to into liner for polytetrafluoroethyl-ne
In the 50mL reactors of alkene, the packing ratio of hydrothermal reaction kettle is 80%, seals hydrothermal reaction kettle；Hydrothermal reaction kettle is put into into baking oven
In, 24h is incubated from room temperature to after 180 DEG C, then naturally cools to room temperature；After by product centrifugation in hydrothermal reaction kettle,
Deionized water and dehydrated alcohol are washed 2 times respectively, are dried 12h at 80 DEG C, you can obtain NaGd (MoO4) 2:Eu3+ is compared with bead
Shape particle light-emitting powder.
Embodiment 6：The Eu (NO3) 3 for measuring the 27.0mlGd (NO3) 3 and 3.0ml of 0.1mol/L concentration respectively is dissolved in beaker
In, mix；It is 1 according to rare earth ion and sodium citrate mol ratio:1.5 add sodium citrate in mixed solution, treat lemon
After lemon acid sodium dissolving, then continuing magnetic force stirring 30min under room temperature is weighed in the above-mentioned mixed solution of 0.7945g sodium molybdate addition
After all dissolving, it is 6 to adjust solution ph with HNO3 and NaOH, continues stirring 30min；Mixed solution is transferred to into liner for poly- four
In the 50mL reactors of fluorothene, the packing ratio of hydrothermal reaction kettle is 80%, seals hydrothermal reaction kettle；Hydrothermal reaction kettle is put into
In baking oven, 24h is incubated from room temperature to after 180 DEG C, then naturally cools to room temperature；Product in hydrothermal reaction kettle is centrifuged
Afterwards, deionized water and dehydrated alcohol are washed 2 times respectively, are dried 12h at 80 DEG C, you can obtain NaGd (MoO4) 2:Eu3+ is larger
Similar spheroidal particle luminescent powder.
The structure and performance that each example of correspondence enforcement obtains product is further analyzed.
From figure 3, it can be seen that preparing NaGd (MoO4) 2:The diffraction maximum of Eu3+ luminescent powders all with PDF cards（JCPDS
NO.25-0828）It is consistent, it is 2 crystalline phases of NaGd (MoO4) of tetragonal crystal system.
As can be seen from Figure 4：NaGd(MoO4)2:The emissive porwer of Eu3+ luminescent powders is related to the pattern of sample.
Claims (7)
1. a kind of morphology controllable NaGd (MoO4)2:Eu3+The preparation method of luminescent powder, it is characterised in that methods described is with Gd2O3
(99.99%), Eu2O3(99.99%), analytically pure sodium molybdate（Na2MoO4•2H2O）With analytically pure sodium citrate（C6H5Na3O7•
2H2O）For raw material, from the hydro-thermal method synthetic technology of sodium citrate auxiliary；
Comprise the following steps that：
（1）By Gd2O3And Eu2O3With 1:1 (V/V) nitric acid dissolves, and adds deionized water to be prepared into the compound nitrate mixing of rare earth molten
Liquid；
（2）Add sodium citrate；
（3）Sodium molybdate is added, precursor solution is uniformly mixing to obtain；
（4）Adjust the pH value of presoma；
（5）The precursor solution adjusted after pH value is transferred in the reactor that liner is politef, hydro-thermal reaction is sealed
After kettle, react a few hours under the conditions of preset temperature, reaction naturally cools to room temperature after terminating, and obtains white precipitate；
（6）The white precipitate for generating is taken out, for several times, being dried a few hours under the conditions of preset temperature obtains NaGd for washing
(MoO4)2:Eu3+Luminescent powder.
2. a kind of morphology controllable NaGd (MoO according to claim 14)2:Eu3+The preparation method of luminescent powder, its feature exist
In：Step（1）Middle Eu3+Account for（Gd3++ Eu3+）Mole percent ratio be 2.5-10%.
3. a kind of morphology controllable NaGd (MoO according to claim 14)2:Eu3+The preparation method of luminescent powder luminescent properties,
It is characterized in that：Step（2）In be 1 according to rare earth ion and sodium citrate mol ratio：0.5-2 adds sodium citrate.
4. a kind of pattern that adjusts according to claim 1 strengthens NaGd (MoO4)2:Eu3+The preparation side of luminescent powder luminescent properties
Method, it is characterised in that：Step（3）In be 14 according to rare earth ion and sodium molybdate mol ratio:3 add sodium molybdate.
5. a kind of morphology controllable NaGd (MoO according to claim 14)2:Eu3+The preparation method of luminescent powder luminescent properties,
It is characterized in that：Step（4）Middle employing HNO3It is 5-7 that pH value is adjusted with NaOH.
6. a kind of morphology controllable NaGd (MoO according to claim 14)2:Eu3+The preparation method of luminescent powder luminescent properties,
It is characterized in that：Step（5）Default reaction temperature is 170-190 DEG C, and sufficient reaction time is 20-48h.
7. a kind of morphology controllable NaGd (MoO according to claim 14)2:Eu3+The preparation method of luminescent powder luminescent properties,
It is characterized in that：Step（6）60-80 DEG C of baking temperature, time are 12-24h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109266347A (en) * | 2018-11-23 | 2019-01-25 | 陕西科技大学 | It is a kind of can be by red fluorescence powder and preparation method thereof that blue chip effectively excites |
| CN109911937A (en) * | 2019-02-01 | 2019-06-21 | 渤海大学 | A kind of NaRE (MoO4)2From sacrifice method for preparing template |
| CN113860388A (en) * | 2021-09-15 | 2021-12-31 | 辽宁大学 | Sodium citrate-assisted synthesis cobalt tungstate material and preparation method and application thereof |
-
2016
- 2016-09-19 CN CN201610830491.1A patent/CN106544019A/en active Pending
Non-Patent Citations (3)
| Title |
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| BI WENBO: "Luminescent properties and energy transfer mechanism of NaGd(MoO4)2:Sm3+, Eu3+ phosphors", 《CERAMICS INTERNATIONAL》 * |
| LI ANMING: "Facile morphology-controllable hydrothermal synthesis and color tunable luminescence properties of NaGd(MoO4)(2):Eu3+,Tb3+ microcrystals", 《RSC ADVANCE》 * |
| 王峻: "水热处理对无水碳酸镁微观结构的影响", 《硅酸盐学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109266347A (en) * | 2018-11-23 | 2019-01-25 | 陕西科技大学 | It is a kind of can be by red fluorescence powder and preparation method thereof that blue chip effectively excites |
| CN109911937A (en) * | 2019-02-01 | 2019-06-21 | 渤海大学 | A kind of NaRE (MoO4)2From sacrifice method for preparing template |
| CN109911937B (en) * | 2019-02-01 | 2021-01-22 | 渤海大学 | NaRE (MoO)4)2Preparation method of self-sacrifice template |
| CN113860388A (en) * | 2021-09-15 | 2021-12-31 | 辽宁大学 | Sodium citrate-assisted synthesis cobalt tungstate material and preparation method and application thereof |
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Application publication date: 20170329 |