CN108531181A - A kind of rare earth doping fluorescent powder of anti-bombardment and preparation method thereof - Google Patents
A kind of rare earth doping fluorescent powder of anti-bombardment and preparation method thereof Download PDFInfo
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- CN108531181A CN108531181A CN201810641857.XA CN201810641857A CN108531181A CN 108531181 A CN108531181 A CN 108531181A CN 201810641857 A CN201810641857 A CN 201810641857A CN 108531181 A CN108531181 A CN 108531181A
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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
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Abstract
The invention discloses a kind of rare earth doping fluorescent powder of anti-bombardment and preparation method thereof, which is characterized in that includes the following steps：S1 weighs a certain amount of terbium oxide, europium oxide and yttrium oxide and is separately added into salpeter solution；S2, constant temperature blender with magnetic force, which constantly heats, to be made it dissolve completely；S3 after room temperature is cooled to crystallization, adds quantitative secondary water；S4 tests to solvent for use and raw material, and a certain amount of Eu (NO3) 3 configured and 3 solution of Y (NO3) are taken with corresponding instrument；S5 is mixed in and burns in stove, stirs 20min；S6 weighs Na2MoO4 and is dissolved in a certain amount of deionized water, stirring；S7 mixes the above solution fully, at room temperature after magnetic agitation 30min, moves into reaction kettle；S8 is centrifuged, ultrasonic washing；S9, it is dry, obtain the rare earth doping fluorescent powder of anti-bombardment.The present invention has many advantages, such as high concentration rare earth ion doping and good stability, is a kind of excellent fluorescence host material, and bombardment resistance is strong.
Description
Technical field
The present invention relates to the rare earth doping fluorescent powder and its preparation side of phosphor technologies field more particularly to a kind of anti-bombardment
Method.
Background technology
Being constantly progressive and develop with science and technology, energy and environmental problem is increasingly prominent, energy-saving consumption-reducing be related to it is current
The great realistic problem of human social.In the case of global environmental requirement continuous improvement, energy shortages, promote
People are constantly finding new alternative energy source or energy-efficient material and device.With new material (GaN semiconductors and novel glimmering
Light powder) development, make the white light emitting diode (W-LED) with characteristics such as energy-saving and environmental protection appearance become it is a kind of may be simultaneously
Obtain larger development.
Rare earth ion has its unique property and structure, can absorb the light of a variety of colors from ultraviolet to infrared, from
And the luminescent material of doping with rare-earth ions is allow to emit the light of multi-wavelength.Because rare earth element is in electricity, magnetic, light and biology
Medical aspects etc. have many special performances, have in military, industrial, luminous, biologic medical and agricultural production etc. important
Application value.No matter rare earth element is used as the matrix components of luminescent material, is also used as activator, coactivator, sensitization
The luminescent material of agent or dopant, commonly referred to collectively as rare earth luminescent material.Rare earth luminescent material is generally by matrix and activator group
At, matrix can be the compound of rare earth compound or other non-rare earths, such as molybdate, under action of ultraviolet light, molybdate
Blue can be sent out to sodium yellow spectral line, and pass to the rare earth ion being entrained in molybdic acid salt matrix, be important luminous host
Material, and activator is usually trace doped foreign ion (such as rare earth ion, transition metal ions) serves as the centre of luminescence.It is right
For rare earth luminescent material, it is important that rare earth ion can realize list by adjusting the type and doping of rare earth ion
White light emission in one matrix, and as the new phosphors of new generation of green lighting source white light LEDs, which overcome a variety of face
Existing color reabsorbs between the mixing of color fluorescent powder and color regulates and controls problem.White light LED fluorescent powder to develop novel is opened
Road is warded off.
Invention content
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of rare earth of the anti-bombardment proposed is mixed
Miscellaneous fluorescent powder and preparation method thereof.
To achieve the goals above, present invention employs following technical solutions：
1, a kind of rare earth doping fluorescent powder of anti-bombardment and preparation method thereof, which is characterized in that include the following steps：
S1 weighs a certain amount of terbium oxide, europium oxide and yttrium oxide and is separately added into 1:In the salpeter solution of 1 (V/V)；
S2, constant temperature blender with magnetic force, which constantly heats, to be made it dissolve completely, slowly the extra nitric acid of evaporative removal；
S3 after room temperature is cooled to crystallization, adds quantitative secondary water, is configured to terbium nitrate and europium nitrate solution, and
Yttrium nitrate solution；
S4 tests to solvent for use and raw material, if be concentration and purity needed for experiment, be verified it is errorless after,
A certain amount of Eu (NO3) 3 configured and 3 solution of Y (NO3) are taken with corresponding instrument；
S5 is mixed according to molar ratio and burns in stove, at room temperature magnetic agitation 20min；
S6 weighs Na2MoO4 and is dissolved in a certain amount of deionized water in molar ratio, stirs 20min.
S7 mixes the above solution fully, at room temperature after magnetic agitation 30min, moves into reaction kettle.
S8 is centrifuged, ultrasonic washing, with secondary water washing three times, ethyl alcohol washing three times when ultrasonic washing；
S9 in ethanol by product dissolving is placed it in surface plate, dry, obtains the rare earth doping fluorescent of anti-bombardment
Powder.
Preferably, in the S1, terbium oxide, europium oxide and yttrium oxide weight proportion are respectively 1-20%, 1-55% and 1-
65%.
Preferably, in the S5, Eu (NO3) 3 and 3 solution ratios of Y (NO3) are 1-45% and 1-75%.
Preferably, in described S5, S6 and S7, mixing plant is preferably high-speed shearing machine, rotating speed 1000-3000r/min.
Preferably, in the S7,1-30h is reacted under 150-800 DEG C of hydrothermal condition in reaction kettle.
Preferably, dry to be preferably positioned in thermostatic drying chamber in the S9, dry 1- under the conditions of 50-80 DEG C
24h。
Preferably, in the S9, rare earth doping fluorescent powder chemical constitution is NaY (MoO4) 2:X%Eu3+.
Compared with prior art, the beneficial effects of the invention are as follows：
It is a kind of excellent 1. NY (MoO4) 2 of the present invention has many advantages, such as high concentration rare earth ion doping and good stability
Good fluorescence host material, bombardment resistance are strong.
2. production process of the present invention has, reaction condition is relatively mild, synthesis temperature is low, product particle size and morphology controllable etc.
Advantage, the powder complete crystallization of preparation, is not required to grind, soilless sticking, good dispersion.
3. NaY (MoO4) 2 of the present invention:The most strong excitation peak of Eu3+ is located at 285nm, and most strong emission peak is located at 613nm, because
This, NaY (MoO4) 2:Eu3+ fluorescent powders can be excited effectively by ultraviolet LED launch wavelength, send out bright feux rouges, adjust Eu3+
Doping, NaY (MoO4) 2:The Color tunable control of Eu3+ fluorescent powders.
In the present invention, it is not directed to part in the device and is the same as those in the prior art or can be realized by using the prior art,
The advantages that high concentration rare earth ion doping of the present invention and good stability is a kind of excellent fluorescence host material, anti-bombardment
Property is strong, adjusts the doping of Eu3+, NaY (MoO4) 2:The Color tunable control of Eu3+ fluorescent powders.
Description of the drawings
Fig. 1 is that the structure of the XRD of rare earth doping fluorescent powder of anti-bombardment proposed by the present invention and preparation method thereof a kind of is shown
It is intended to；
Fig. 2 is a kind of emission spectrum structure of rare earth doping fluorescent powder of anti-bombardment proposed by the present invention and preparation method thereof
Schematic diagram.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that, term "upper", "lower", "front", "rear", "left", "right", "top",
The orientation or positional relationship of the instructions such as "bottom", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, merely to just
In the description present invention and simplify description, do not indicate or imply the indicated device or element must have a particular orientation, with
Specific azimuth configuration and operation, therefore be not considered as limiting the invention.
Embodiment 1：A kind of rare earth doping fluorescent powder of anti-bombardment and preparation method thereof, which is characterized in that including following step
Suddenly：S1 weighs a certain amount of terbium oxide, europium oxide and yttrium oxide and is separately added into 1:In the salpeter solution of 1 (V/V)；S2, constant temperature magnetic
Power blender, which constantly heats, to be made it dissolve completely, slowly the extra nitric acid of evaporative removal；S3, after room temperature is cooled to crystallization,
Quantitative secondary water is added, terbium nitrate and europium nitrate solution and yttrium nitrate solution are configured to；S4, to solvent for use and original
Material is tested, if be concentration and purity needed for experiment, be verified it is errorless after, take a certain amount of configuration with corresponding instrument
Good 3 solution of Eu (NO3) 3 and Y (NO3)；S5 is mixed according to molar ratio and burns in stove, at room temperature magnetic agitation 20min；S6,
Na2MoO4 is weighed in molar ratio to be dissolved in a certain amount of deionized water, stirs 20min；The above solution is mixed abundant, room by S7
After the lower magnetic agitation 30min of temperature, move into reaction kettle；S8 is centrifuged, ultrasonic washing, with secondary when ultrasonic washing
Water washing three times, ethyl alcohol wash three times；S9 in ethanol by product dissolving is placed it in surface plate, dry, obtains anti-bang
The rare earth doping fluorescent powder hit.
In the S1, terbium oxide, europium oxide and yttrium oxide weight proportion are respectively 18%, 35% and 60%；In the S5,
Eu (NO3) 3 and 3 solution ratios of Y (NO3) are 35% and 65%；In described S5, S6 and S7, mixing plant is preferably high speed shear
Machine, rotating speed 2000r/min；In the S7,15h is reacted under 300 DEG C of hydrothermal condition in reaction kettle；In the S9, drying is excellent
It is selected as being positioned in thermostatic drying chamber, dry 13h under the conditions of 70 DEG C；In the S9, rare earth doping fluorescent powder chemical constitution is
NaY(MoO4)2:X%Eu3+.
Experiment measures：Fig. 1 is the NaY (MoO4) 2 prepared:The XRD diagram of 11%Tb3+, it can be seen that all diffraction maximum with
PDF#82-2369 (NaY (MoO4) 2) standard card is corresponding.It follows that sample diffraction figure prepared by the Tb3+ of various concentration
Compose closely similar, the position of diffraction maximum has almost no change.Main diffraction maximum is very strong and sharp as seen from the figure, almost without extra
Dephasign, it is seen that crystal growth is good, and the Tb3+ ions adulterated on a small quantity do not influence the crystal phase structure of NaY (MoO4) 2.
Embodiment 2：A kind of rare earth doping fluorescent powder of anti-bombardment and preparation method thereof, which is characterized in that including following step
Suddenly：S1 weighs a certain amount of terbium oxide, europium oxide and yttrium oxide and is separately added into 1:In the salpeter solution of 1 (V/V)；S2, constant temperature magnetic
Power blender, which constantly heats, to be made it dissolve completely, slowly the extra nitric acid of evaporative removal；S3, after room temperature is cooled to crystallization,
Quantitative secondary water is added, terbium nitrate and europium nitrate solution and yttrium nitrate solution are configured to；S4, to solvent for use and original
Material is tested, if be concentration and purity needed for experiment, be verified it is errorless after, take a certain amount of configuration with corresponding instrument
Good 3 solution of Eu (NO3) 3 and Y (NO3)；S5 is mixed according to molar ratio and burns in stove, at room temperature magnetic agitation 20min；S6,
Na2MoO4 is weighed in molar ratio to be dissolved in a certain amount of deionized water, stirs 20min；The above solution is mixed abundant, room by S7
After the lower magnetic agitation 30min of temperature, move into reaction kettle；S8 is centrifuged, ultrasonic washing, with secondary when ultrasonic washing
Water washing three times, ethyl alcohol wash three times；S9 in ethanol by product dissolving is placed it in surface plate, dry, obtains anti-bang
The rare earth doping fluorescent powder hit.
In the S1, terbium oxide, europium oxide and yttrium oxide weight proportion are respectively 20%, 50% and 55%；In the S5,
Eu (NO3) 3 and 3 solution ratios of Y (NO3) are 40% and 70%；In described S5, S6 and S7, mixing plant is preferably high speed shear
Machine, rotating speed 2400r/min；In the S7,5h is reacted under 600 DEG C of hydrothermal condition in reaction kettle；It is dry preferred in the S9
To be positioned in thermostatic drying chamber, dry 6h under the conditions of 80 DEG C；In the S9, rare earth doping fluorescent powder chemical constitution is NaY
(MoO4)2:X%Eu3+.
Experiment measures：Fig. 2 is the launching light spectrogram under the excitation of 279nm wavelength.Three transmittings under the excitation of phase co-wavelength
The position at peak is essentially identical, and respectively at 490nm, 545nn, 587nm, the emission peak of these points is all the 4f shell electricity by Tb3+
Caused by the f-f transition of son, 5D4 → 7F6 (490nm), 5D4 → 7F5 (545nm), 5D4 → 7F4 (587nm) are corresponded respectively to
Transition transmitting, wherein highest peak is located at 545nm.With the increase of doping Tb3+ concentration, characteristic emission peak intensity gradually increases
Add.We from illustration it can also be seen that with Tb3+ doping concentrations increase, characteristic emission (545nm) intensity of Tb3+ by
It is cumulative strong.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of rare earth doping fluorescent powder of anti-bombardment and preparation method thereof, which is characterized in that include the following steps：
S1 weighs a certain amount of terbium oxide, europium oxide and yttrium oxide and is separately added into 1:In the salpeter solution of 1 (V/V)；
S2, constant temperature blender with magnetic force, which constantly heats, to be made it dissolve completely, slowly the extra nitric acid of evaporative removal；
S3 after room temperature is cooled to crystallization, adds quantitative secondary water, is configured to terbium nitrate and europium nitrate solution and nitric acid
Yttrium solution；
S4 tests to solvent for use and raw material, if be concentration and purity needed for experiment, be verified it is errorless after, use phase
The instrument answered takes a certain amount of Eu (NO3) 3 configured and 3 solution of Y (NO3)；
S5 is mixed according to molar ratio and burns in stove, at room temperature magnetic agitation 20min；
S6 weighs Na2MoO4 and is dissolved in a certain amount of deionized water in molar ratio, stirs 20min；
S7 mixes the above solution fully, at room temperature after magnetic agitation 30min, moves into reaction kettle；
S8 is centrifuged, ultrasonic washing, with secondary water washing three times, ethyl alcohol washing three times when ultrasonic washing；
S9 in ethanol by product dissolving is placed it in surface plate, dry, obtains the rare earth doping fluorescent powder of anti-bombardment.
2. a kind of rare earth doping fluorescent powder and preparation method thereof of anti-bombardment according to claim 1, which is characterized in that institute
It states in S1, terbium oxide, europium oxide and yttrium oxide weight proportion are respectively 1-20%, 1-55% and 1-65%.
3. a kind of rare earth doping fluorescent powder and preparation method thereof of anti-bombardment according to claim 1, which is characterized in that institute
It states in S5, Eu (NO3) 3 and 3 solution ratios of Y (NO3) are 1-45% and 1-75%.
4. a kind of rare earth doping fluorescent powder and preparation method thereof of anti-bombardment according to claim 1, which is characterized in that institute
It states in S5, S6 and S7, mixing plant is preferably high-speed shearing machine, rotating speed 1000-3000r/min.
5. a kind of rare earth doping fluorescent powder and preparation method thereof of anti-bombardment according to claim 1, which is characterized in that institute
It states in S7, reacts 1-30h under 150-800 DEG C of hydrothermal condition in reaction kettle.
6. a kind of rare earth doping fluorescent powder and preparation method thereof of anti-bombardment according to claim 1, which is characterized in that institute
It states in S9, dry to be preferably positioned in thermostatic drying chamber, dry 1-24h under the conditions of 50-80 DEG C.
7. a kind of rare earth doping fluorescent powder and preparation method thereof of anti-bombardment according to claim 1, which is characterized in that institute
It states in S9, rare earth doping fluorescent powder chemical constitution is NaY (MoO4) 2:X%Eu3+.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115820246A (en) * | 2022-11-21 | 2023-03-21 | 桂林电子科技大学 | Preparation method and application of rare earth terbium-doped gallium oxide fluorescent material |
| CN117143601A (en) * | 2023-08-16 | 2023-12-01 | 东台市天源光电科技有限公司 | Color-adjustable nano rare earth anti-counterfeiting fluorescent powder and preparation method thereof |
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| CN105038791A (en) * | 2015-06-23 | 2015-11-11 | 西安建筑科技大学 | Preparation method of spherical red phosphor powder capable of being excited by ultraviolet-blue light |
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2018
- 2018-06-21 CN CN201810641857.XA patent/CN108531181A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105038791A (en) * | 2015-06-23 | 2015-11-11 | 西安建筑科技大学 | Preparation method of spherical red phosphor powder capable of being excited by ultraviolet-blue light |
Non-Patent Citations (4)
| Title |
|---|
| LIU HAI-YAN ET AL.,: ""Photoluminescence properties of solid-state Tb3+ doped NaY(MoO4)2"", 《OPTOELECTRONICS LETTERS》 * |
| YING LI ET AL.,: ""Formation and down/up conversion luminescence of Ln3+ doped NaY(MoO4)2 microcrystals"", 《DALTON TRANS》 * |
| ZHENHE XU ET AL.,: ""Self-Assembled 3D Urchin-Like NaY(MoO4)2:Eu3+/Tb3+ Microarchitectures: Hydrothermal Synthesis and Tunable Emission Colors"", 《J. PHYS. CHEM. C》 * |
| 王雅静 等: ""Eu3+,Tb3+共掺杂NaY（MoO4）2材料的制备及发光性能研究"", 《电子元件与材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115820246A (en) * | 2022-11-21 | 2023-03-21 | 桂林电子科技大学 | Preparation method and application of rare earth terbium-doped gallium oxide fluorescent material |
| CN117143601A (en) * | 2023-08-16 | 2023-12-01 | 东台市天源光电科技有限公司 | Color-adjustable nano rare earth anti-counterfeiting fluorescent powder and preparation method thereof |
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Application publication date: 20180914 |