CN109233822A - A kind of yellow longpersistent luminescent material and its preparation method and application - Google Patents
A kind of yellow longpersistent luminescent material and its preparation method and application Download PDFInfo
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- CN109233822A CN109233822A CN201811094261.9A CN201811094261A CN109233822A CN 109233822 A CN109233822 A CN 109233822A CN 201811094261 A CN201811094261 A CN 201811094261A CN 109233822 A CN109233822 A CN 109233822A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- C09K11/7707—Germanates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- C09K11/7793—Germanates
Abstract
The present invention provides a kind of yellow longpersistent luminescent material, is related to novel inorganic field of functional materials.A kind of yellow longpersistent luminescent material, which is characterized in that using germanium barium stannate as luminescent material substrate, with trivalent rare earth ions Dy3+For activator, the expression formula of the yellow longpersistent luminescent material are as follows: Ba1‑xSnGe3O9: xDy3+Or Ba1‑x‑ySnGe3O9:xDy3+,yRe；Wherein, Re is selected from La3+、Ce3+、Pr3+、Nd3+、Sm3+、Eu3+、Gd3+、Tb3+、Ho3+、Yb3+、Lu3+、Er3+One of or it is a variety of；0.0005≤x≤0.05,0.0005≤y≤0.05.The capable of emitting naked eyes visible yellow color twilight sunset of the material has stronger afterglow intensity, and decay of afterglow is slower, and persistence is longer.The present invention also provides preparation method, preparation process is simple, condition is easily-controllable, equipment requirement is low, generates in preparation process without toxic gas, no pollution to the environment.
Description
Technical field
The present invention relates to novel inorganic field of functional materials, and in particular to a kind of yellow longpersistent luminescent material and its system
Preparation Method and application.
Background technique
Long-persistence luminous (Long persistence luminescence) refers to after removing excitaton source, still can be with
Several minutes of the continuous illumination optical phenomenas to a few hours, process are broadly divided into energy absorption, and energy storage and energy release are
The afterglow stage.Long afterglow phenomenon is early just to be observed and is recorded by people in ancient times, but until modern age people just start gradually
Understanding studies its luminescence phenomenon and luminescence mechanism.And since its is environmentally friendly, equal excellent characteristics, long afterglow hair can be recycled
In recent years by the concern of people, research and development is grown rapidly luminescent material.Long-afterglow material is a kind of New Energy
Amount storage and electron capture material, it can be adulterated different after absorbing energy capture electronics in continuous illumination under low light environment
Rare earth ion or transition metal ions etc., can produce the transition of different energy levels to issue the light of various wave bands, meet not
The demand of same domain, it cannot only be applied to the traditional fields such as Emergency Light and display, also can be applied to high-energy ray spy
The high and new technologies field such as survey, fibre optic thermometer, the lossless detection of engineering ceramics and ultra high density optical storage and display, in life
Object in-vivo imaging, the fields such as lesion detection also have potential application.
So far, people oneself developed a variety of long after glow luminous material that can issue different colours light.For example, hair
Green light SrAl out2O4:Eu2+,Dy3+, issue blue light CaAl2O4:Eu2+,Nd3+, issue blue light Sr4Al14O25:Eu2+,Dy3+, issue
The Zn of feux rouges3Ga2Ge2O10:Cr3+.Wherein, best performance is good and the long-afterglow material that has put it into commercial operation is SrAl2O4:Eu2+,Dy3 +, because it is with stronger afterglow intensity and persistence duration duration.But SrAl2O4:Eu2+,Dy3+It is chemical under air atmosphere
Property is not sufficiently stable, and is easily deliquesced.Therefore, develop that a kind of chemical property is stable, nontoxic and preparation method is simple in this field
Long after glow luminous material, research to material and apply very big driving force.
Summary of the invention
The purpose of the present invention is to provide a kind of yellow longpersistent luminescent materials, this long after glow luminous material is in low light environment
Under, capable of emitting naked eyes visible yellow color twilight sunset has stronger afterglow intensity and afterglow duration.
Another object of the present invention is to provide a kind of preparation method of yellow longpersistent luminescent material, preparation process letters
It is single, condition is easy to control, equipment requirement is low, is generated in preparation process without toxic gas, no pollution to the environment.
The present invention solves its technical problem and adopts the following technical solutions to realize.
A kind of yellow longpersistent luminescent material, using germanium barium stannate as luminescent material substrate, with trivalent rare earth ions Dy3+For
Activator, the expression formula of the yellow longpersistent luminescent material are as follows: Ba1-xSnGe3O9: xDy3+Or Ba1-x-ySnGe3O9:xDy3+,
yRe；Wherein, Re is selected from La3+、Ce3+、Pr3+、Nd3+、Sm3+、Eu3+、Gd3+、Tb3+、Ho3+、Yb3+、Lu3+、Er3+One of or
It is a variety of；0.0005≤x≤0.05,0.0005≤y≤0.05.
The present invention also proposes a kind of preparation method of yellow longpersistent luminescent material, comprising the following steps:
S1 weighs compound containing Ba, compound containing Sn, containing Geization according to the molar ratio of each element in the expression formula respectively
Object, compound containing Dy and compound containing Re are closed, by above-mentioned weighed each raw material mixed grinding, raw material powder is made；
The raw material powder is carried out first time calcining, grinds after cooling and obtain being pre-sintered sample by S2；
S3, carries out second for the pre-sintering sample and calcines, grind after cooling, and then crossing sieve, to obtain the yellow long
Afterglow materials powder.
A kind of beneficial effect of yellow longpersistent luminescent material of the present invention and preparation method thereof is:
(1) present invention prepares long after glow luminous material using traditional solid phase method, preparation process is simple, condition is easily-controllable,
Equipment requirement is low and raw material Ba, Sn, Ge be it is tellurian belong to environmentally protective environmentally friendly material rich in element, prepare
It is generated in the process without toxic gas, no pollution to the environment.The germanium barium stannate being prepared is under atmospheric atmosphere, compared to common aluminium
Hydrochlorate has higher stability, is not susceptible to deliquesce.Therefore, use germanium barium stannate as the preparation-obtained long afterglow material of substrate
Expect that chemical property is more stable.
(2) the yellow longpersistent luminescent material Ba obtained by the present invention1-xSnGe3O9: xDy3+It is placed under ultraviolet lamp and excites one
After the section time, under low light environment, capable of emitting naked eyes visible yellow color twilight sunset, emission peak has stronger remaining in 580nm or so
Brightness intensity, decay of afterglow is slower, and persistence is longer.
(3) yellow longpersistent luminescent material Ba produced by the present invention1-x-ySnGe3O9:xDy3+, in yRe, Dy3+It is co-doped with other
Different ions, such as La3+、Ce3+、Pr3+、Nd3+、Sm3+、Eu3+、Gd3+、Tb3+、Ho3+、Yb3+、Lu3+、Er3+In wherein one
Kind is a variety of, increases the carrier traps number in base material by the doping of different elements or changes the hair of sample
Optical band.
(4) film that can be mixed with organic high score material of yellow longpersistent luminescent material prepared by the present invention or
Resinite is it in Emergency Light, opto-electronic device or member as light-emitting film or the luminescent device with yellow twilight sunset
Part, instrument show etc. that the practical application in fields lays the foundation.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is a kind of preparation flow figure of yellow longpersistent luminescent material provided in an embodiment of the present invention；
Fig. 2 is the X ray diffracting spectrum of yellow longpersistent luminescent material prepared by the embodiment of the present invention 1~5；
Fig. 3 is the emission spectrum of the long after glow luminous material of yellow twilight sunset prepared by the embodiment of the present invention 3；
Fig. 4 is the yellow longpersistent luminescent material twilight sunset spectrum for preparing in the Examples 1 to 5 of material of the present invention.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
A kind of yellow longpersistent luminescent material of the embodiment of the present invention and preparation method thereof is specifically described below.
A kind of yellow longpersistent luminescent material provided in an embodiment of the present invention, using germanium barium stannate as luminescent material substrate,
With trivalent rare earth ions Dy3+For activator, the expression formula of the yellow longpersistent luminescent material are as follows: Ba1-xSnGe3O9: xDy3+Or
Ba1-x-ySnGe3O9:xDy3+,yRe；Wherein, Re is selected from La3+、Ce3+、Pr3+、Nd3+、Sm3+、Eu3+、Gd3+、Tb3+、Ho3+、Yb3+、
Lu3+、Er3+One of or it is a variety of；0.0005≤x≤0.05,0.0005≤y≤0.05.Wherein, x, y indicate that Mole percent contains
Amount.The present invention is using germanium barium stannate material as substrate, using trivalent rare earth ions Dy3+For activator, by singly mixing Dy3+In substrate
Middle formation trap captures free electron, can also be by La3+、Ce3+、Pr3+、Nd3+、Sm3+、Eu3+、Gd3+、Tb3+、Ho3+、Yb3+、Lu3+、
Er3+One of or a variety of and Dy3+Codope increases the carrier traps in base material by the doping of different elements
Number or the luminescence band for changing sample so that the yellow longpersistent luminescent material prepared have stronger afterglow intensity and
Persistence duration duration, and macroscopic afterglow is generated, it is that it is aobvious in Emergency Light, opto-electronic device or element, instrument
Show that the practical application in equal fields lays the foundation.
Further, the ratio of the x and the y are 1:0.5~1.5.It is further preferable that the ratio of x and y is 1:1.Control
The ratio of x and y processed, guarantee have sufficient concentrations of Dy3+Ion, as activator and the centre of luminescence.It avoids Re element excessive, prepares
Obtained long-afterglow material is impure, and long-afterglow material illumination effect is caused to decline.Wherein, the optimum proportioning of x is 0.02.
The preparation method for the above-mentioned yellow longpersistent luminescent material that the embodiment of the present invention also provides, comprising the following steps:
S1 weighs compound containing Ba, compound containing Sn, containing Geization according to the molar ratio of each element in the expression formula respectively
Object, compound containing Dy and compound containing Re are closed, by above-mentioned weighed each raw material mixed grinding, raw material powder is made.
Further, in step sl, above-mentioned each raw material is selected from the mixing of oxide containing corresponding element, salt or both
Object；Wherein, the salt is selected from nitrate and/or carbonate.In a preferred embodiment of the present invention, it can be selected in compound containing Ba
Oxide, nitrate or carbonate then select its oxide containing Sn and compound containing Ge, then select it containing Dy and compound containing Re
Oxide or nitrate.
Preferably, in an embodiment of the present invention, BaCO is selected3、SnO2、GeO2、Dy2O3As Material synthesis raw material, on
It states raw material to be easy to obtain, and relative low price.And Ba, Sn, Ge are tellurian rich in element, belong to environmentally protective environment
Friendly material, the finished product no pollution to the environment being prepared.
Further, in step sl, grinding steps are as follows: will compound containing Ba, compound containing Sn, the chemical combination containing Ge
Solvent is added after object, compound containing Dy and the mixing of compound containing Re and grinds 1~4h.Wherein the solvent be dehydrated alcohol, water or
The mixture of the two.By each raw material mixed grinding, each element is made to be evenly distributed, it is abundant to be conducive to subsequent step reaction.Second is added
Alcohol or water are ground, and are conducive to grinding more evenly, and do not react with raw material.
The raw material powder is carried out first time calcining, grinds after cooling and obtain being pre-sintered sample by S2.
The raw material powder is warming up to 700~1000 DEG C in air atmosphere with the speed of 1~10 DEG C/min, calcination 2
Room temperature is naturally cooled to furnace after being cooled to 200~500 DEG C after~4 hours with the rate of temperature fall of 5~15 DEG C/min, is obtained described
It is pre-sintered sample.
Further, raw material powder is warming up to 750~850 DEG C in air atmosphere with the speed of 2~5 DEG C/min,
Obtain the pre-sintering sample within calcination 2~4 hours.Heating rate is controlled, is conducive to not react because of excessive temperature differentials between raw material
It is uneven.It is further preferable that being heated up with the heating rate of 5 DEG C/min.
Further, it carries out naturally cooling to room temperature with furnace after being cooled to 200~300 DEG C with 10~15 DEG C/min.Control
Annealing temperature processed is conducive to reaction temperature rapid decrease, shortens experimental period, avoids annealing time too long, product is caused to move back
Fiery process continues sintering and grows up.
S3, carries out second for the pre-sintering sample and calcines, grind after cooling, and then crossing sieve, to obtain the yellow long
Afterglow materials powder.
Further, in step s3, second the step of calcining are as follows: by the pre-sintering sample in air atmosphere with
The speed of 1~10 DEG C/min is warming up to 1200~1400 DEG C, calcination 3~8 hours.
Further, raw material powder is warming up to 1200~1400 in air atmosphere with the speed of 4~8 DEG C/min
DEG C, calcination 5~8 hours.Above-mentioned condition keeps reaction more abundant, and is unlikely to keep temperature-rise period excessively slow.
Using first calcining, rear grinding, the again method calcined, it is able to suppress product and occurs to be sintered in calcination process and grow up,
Guarantee that sufficiently, the product component of preparation is pure, and the long after glow luminous material powder prepared is more thin for reaction in calcination process
It is greasy.And calcination atmosphere is only air atmosphere twice, reaction of not appraising at the current rate in reaction process, therefore compares and carried out with reducing atmosphere
For the prior art of calcining, cost is relatively low, more advantageous.
Further, in step s3, the mesh number of the sieve is 20~50 mesh.Sieve is carried out to the powder of preparation arrived
Filtering, guarantees that the long after glow luminous material powder diameter being prepared is consistent, uniformly, fine and smooth.
Further, further include the steps that sealing the yellow longpersistent luminescent material powder up for safekeeping:
S4, the film or resinite that the yellow longpersistent luminescent material powder and organic high score material are mixed.
Organic high score material such as the yellow longpersistent luminescent material powder being prepared and silica gel, resin can be mixed film or
Person's resinite realizes the transmitting and storage of luminous energy.
The embodiment of the present invention provides a kind of yellow longpersistent luminescent material, can be in the dark with remaining under the excitation of ultraviolet lamp
Brightness form shines, and afterglow intensity can be visually noticeable.And decay of afterglow is slower, twilight sunset launch time, sustainable number was small
When.These characteristics can be such that yellow longpersistent luminescent material is shown in meet an urgent need indicating device, opto-electronic device, instrument of night applying
In the fields such as device, illuminating device, family adornment.
Feature and performance of the invention are described in further detail with reference to embodiments.
Examples 1 to 6
Examples 1 to 6 provides a kind of yellow longpersistent luminescent material respectively, and preparation step is as follows:
(1) raw material that according to the form below weighs each element is mixed, and dehydrated alcohol is added and carries out being fully ground 3h, obtains original
Feed powder end.
(2) raw material powder is placed in high temperature process furnances, in air atmosphere, is warming up to 800 with the speed of 5 DEG C/min
DEG C, room temperature is naturally cooled to furnace after dropping to 200 DEG C after calcination 2 hours with 10 DEG C/min, obtains being pre-sintered sample.
(3) it takes out after being fully ground, is placed in high temperature process furnances again, in air after being pre-sintered sample and being cooled to room temperature
Under atmosphere, it is warming up to after 1300 DEG C, calcination 4 hours with the speed of 7 DEG C/min and naturally cools to room temperature with furnace.
(4) it is sieved after regrinding cooling sample in 20~50 mesh screens, obtains yellow longpersistent luminescent material.
(5) yellow longpersistent luminescent material powder is fitted into cuvette, its light can be tested after ultraviolet excitation
Learn performance.
Bottom vertical line is pure phase BaSnGe in figure3O9Peak, and yellow longpersistent that Examples 1 to 5 is prepared shines
The diffraction maximum and pure phase BaSnGe of material3O9Diffraction maximum be consistent, do not detect the Dy of doping3+Other phases, show
The sample of preparation has the characteristics that high-purity, and doping with rare-earth ions Dy3+Do not upset crystal structure.
Fig. 3 is the emission spectrum of the long after glow luminous material of yellow twilight sunset prepared by the embodiment of the present invention 3.It can be in figure
Find out that emission peak is located at 490nm, is Dy at 580nm, 680nm3+Characteristic emission peak, it can be seen that Dy3+In luminescent material base
It is as the centre of luminescence in bottom.
Fig. 4 is the yellow longpersistent luminescent material twilight sunset spectrum for preparing in the Examples 1 to 5 of material of the present invention.From figure
It can press out, the twilight sunset transmitting top of Examples 1 to 5 is shown as yellow twilight sunset, belongs to Dy in 580nm or so3+'s4F9/2
It arrives6H13/2Energy level transition.And Examples 1 to 5 all has stronger twilight sunset emissive porwer.Wherein, embodiment 3 is with respect to other implementations
For example, twilight sunset emissive porwer is strongest.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, 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.
Claims (10)
1. a kind of yellow longpersistent luminescent material, which is characterized in that using germanium barium stannate as luminescent material substrate, with trivalent rare earth
Ion Dy3+For activator, the expression formula of the yellow longpersistent luminescent material are as follows: Ba1-xSnGe3O9: xDy3+Or Ba1-x- ySnGe3O9:xDy3+,yRe；Wherein, Re is selected from La3+、Ce3+、Pr3+、Nd3+、Sm3+、Eu3+、Gd3+、Tb3+、Ho3+、Yb3+、Lu3+、
Er3+One of or it is a variety of；0.0005≤x≤0.05,0.0005≤y≤0.05.
2. yellow longpersistent luminescent material according to claim 1, which is characterized in that the ratio of the x and the y are 1:
0.5~1.5.
3. a kind of preparation method of the yellow longpersistent luminescent material as described in claim 1~2 any one, feature exist
In, comprising the following steps:
S1 weighs compound containing Ba, compound containing Sn, chemical combination containing Ge according to the molar ratio of each element in the expression formula respectively
Raw material powder is made in above-mentioned weighed each raw material mixed grinding by object, compound containing Dy and compound containing Re；
The raw material powder is carried out first time calcining, grinds after cooling and obtain being pre-sintered sample by S2；
S3, carries out second for the pre-sintering sample and calcines, grind after cooling, then crosses sieve and obtains the yellow longpersistent
Luminescent material powder.
4. the preparation method of yellow longpersistent luminescent material according to claim 3, which is characterized in that in step sl,
Above-mentioned each raw material is selected from the mixture of oxide containing corresponding element, salt or both；Wherein, the salt be nitrate and/
Or carbonate.
5. the preparation method of yellow longpersistent luminescent material according to claim 3, which is characterized in that in step sl,
Grinding steps are as follows:
It is added after the compound containing Ba, compound containing Sn, compound containing Ge, compound containing Dy and compound containing Re are mixed molten
1~4h is ground in agent；Wherein the solvent is the mixture of dehydrated alcohol, water or both.
6. the preparation method of yellow longpersistent luminescent material according to claim 3, which is characterized in that in step s 2,
The step of calcining for the first time are as follows:
The raw material powder is warming up to 700~1000 DEG C in air atmosphere with the speed of 1~10 DEG C/min, calcination 2~4 is small
When after be cooled to 200~500 DEG C with the rate of temperature fall of 5~15 DEG C/min after naturally cool to room temperature with furnace, obtain the pre-burning
Tie sample.
7. the preparation method of yellow longpersistent luminescent material according to claim 3, which is characterized in that in step s3,
The step of second of calcining are as follows:
The pre-sintering sample is warming up to 1200~1400 DEG C in air atmosphere with the speed of 1~10 DEG C/min, calcination 3~
8 hours.
8. the preparation method of yellow longpersistent luminescent material according to claim 3, which is characterized in that in step s3,
The mesh number of the sieve is 20~50 mesh.
9. the preparation method of yellow longpersistent luminescent material according to claim 3, which is characterized in that further include sealing institute up for safekeeping
The step of stating yellow longpersistent luminescent material powder:
S4, the film or resinite that the yellow longpersistent luminescent material powder and high-molecular organic material are mixed.
10. yellow longpersistent luminescent material as described in claim 1~2 any one production night emergency indicating device,
Opto-electronic device, instrument display part, illuminating device, the application in family adornment.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115340864A (en) * | 2022-09-15 | 2022-11-15 | 厦门理工学院 | Red luminescent material and preparation method and application thereof |
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| CN103131415A (en) * | 2013-03-05 | 2013-06-05 | 中山大学 | Yellow long-lasting phosphor material and preparation method thereof |
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| CN103131415A (en) * | 2013-03-05 | 2013-06-05 | 中山大学 | Yellow long-lasting phosphor material and preparation method thereof |
| CN106497555A (en) * | 2016-11-01 | 2017-03-15 | 兰州大学 | Long persistence luminescent silicate material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115340864A (en) * | 2022-09-15 | 2022-11-15 | 厦门理工学院 | Red luminescent material and preparation method and application thereof |
| CN115340864B (en) * | 2022-09-15 | 2023-08-25 | 厦门理工学院 | Red luminescent material and preparation method and application thereof |
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