CN107129801A - A kind of Li+The method for being co-doped with improving silicate fluorescent powder long afterglow property - Google Patents
A kind of Li+The method for being co-doped with improving silicate fluorescent powder long afterglow property Download PDFInfo
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- CN107129801A CN107129801A CN201710231586.6A CN201710231586A CN107129801A CN 107129801 A CN107129801 A CN 107129801A CN 201710231586 A CN201710231586 A CN 201710231586A CN 107129801 A CN107129801 A CN 107129801A
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- 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
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Abstract
The present invention provides one kind Li+It is co-doped with effectively improving Sr2MgSi2O7:xEu2+,yDy3+Fluorescent material sunset glow intensity and the method for sunset glow time.Work as Li+When being co-doped with, Li+Sr can be replaced2+Case formation Li ‵SrAnd with monovalence negative electrical charge, so positively charged Lacking oxygen can be produced accordingly to supply charge differences, and the Lacking oxygen produced can capture electronics and hole in excitation state as trap, due to heat energy, captured electronics and hole can gradually be discharged, both recombine, and phosphorescence are discharged, here it is long afterglow.And with Li+Doping, Lacking oxygen constantly increases, and captured electronics is also continuously increased, and thus effectively raises the long afterglow time.In addition, Li+Charge compensation is made, makes trivalent Dy3+Replace divalence Sr2+When electric charge be compensated balance.Li+Fluxing agent can also be made, can effectively improve the crystallinity of crystal and expand the particle size of crystal, so as to improve crystallization, long-persistence luminous intensity is finally improved.
Description
Technical field
The invention belongs to rare earth luminescent material technical field, and in particular to a kind of Li+It is co-doped with improving silicate fluorescent
The method of powder long afterglow property, more precisely provides one kind by being co-doped with Li+Improve Sr2MgSi2O7:xEu2+,yDy3+Fluorescent material
The method of long afterglow property.
Background technology
Long lad phosphor is also known as luminous storage fluorescence powder, and it is substantially a kind of embedded photoluminescent material, and he is that a class absorbs
Energy such as visible ray, ultraviolet light, X-ray etc., and excite stop after may continue to send the material of light at room temperature, he can be by
Energy storage is a kind of material with application prospect in it can fall into.Fluorescent material with the lasting characteristics of luminescence is environmental protection and energy
Enough materials by the economy of energy, in safety sign, have wide application prospect on traffic sign and self luminous technics.
The long after glow luminous material used at present mainly has three major types：One class is that traditional sulfide series is long-persistence luminous
Material a, class is aluminates system long after glow luminous material, and the 3rd class is silicate systems long after glow luminous material.With it is traditional
Sulfide long-afterglow material is compared, and aluminates system long after glow luminous material has after-glow brightness high, the advantage of twilight sunset length, and right
Health and environment are all without generation harm.But this kind of materials water-resistant is poor, physical chemistry need to be carried out in particle surface and repaiied
Decorations, to improve its stability, and the long afterglow performance of blue-light-emitting is not good, and the luminous material of aluminate is limited to a certain extent
The application of material.And silicate systems luminescent material as a kind of new long after glow luminous material in recent years increasingly by people
Concern.Compared with traditional aluminates system and sulfide systems, silicate systems have more preferable chemical stability, heat
Stability, water resistance is strong, with ceramic matrix compatibility it is good the advantages of, and silica material is inexpensive, be easy to get, silicate systems
Calcining heat is lower than aluminate more than 100 DEG C, thus is with a wide range of applications.And Sr2MgSi2O7:xEu2+,yDy3+It is luminous
Material is the Typical Representative in aluminates system, while being also one of best material of blue-light-emitting long afterglow performance.Current institute
The Sr of preparation2MgSi2O7:xEu2+,yDy3+Long after glow luminous material has a stable chemical performance, the strong advantage of water resistance, still
Overall luminescent properties not yet reach the level of aluminate luminescent material, and which greatly limits Sr2MgSi2O7:
xEu2+,yDy3+Long after glow luminous material is further applied.Therefore, this area can be effectively improved in the urgent need to developing one kind
Sr2MgSi2O7:xEu2+,yDy3+Fluorescent material sunset glow intensity and the method for sunset glow time.
The content of the invention
It is an object of the invention to solve the above problems, there is provided one kind Li+It is co-doped with effectively improving
Sr2MgSi2O7:xEu2+,yDy3+Fluorescent material sunset glow intensity and the method for sunset glow time.Work as Li+When being co-doped with, Li+Sr can be replaced2+Lattice
Position forms Li ‵SrAnd with monovalence negative electrical charge, positively charged Lacking oxygen can be so produced accordingly to supply charge differences, and produce
Raw Lacking oxygen can capture electronics and hole in excitation state, due to heat energy, captured electronics as trap
It can gradually be discharged with hole, both recombine, discharge phosphorescence, here it is long afterglow.And with Li+Doping, oxygen is empty
Position constantly increase, captured electronics is also continuously increased, and thus effectively raises the long afterglow time.In addition, Li+Do electricity
Lotus compensates, and makes trivalent Dy3+Replace divalence Sr2+When electric charge be compensated balance.Li+Fluxing agent can also be made, can effectively be changed
The crystallinity of kind crystal and the particle size for expanding crystal, so as to improve crystallization, finally improve long-persistence luminous intensity.
The purpose of the present invention can be achieved through the following technical solutions：
On the one hand, the present invention provides a kind of method for the long afterglow property for improving silicate fluorescent powder, and this method is to pass through
Li is co-doped with high silicate+To improve silicate fluorescent powder long afterglow property, wherein, Li+It is co-doped with the composition of silicate fluorescent powder
Shown in following formula：
Sr2MgSi2O7:xEu2+yDy3+zLi+
The span of wherein x, y, z be respectively 0.005≤x≤0.03,0.01≤y≤0.05 and 0.015≤z≤
0.03。
On the other hand, the present invention provides one kind and prepares Li+The method of silicate fluorescent powder is co-doped with, this method includes following step
Suddenly：
(1) to contain lithium ion Li+, magnesium ion M2-, strontium ion Sr2+, silicon ion Si4+, europium ion Eu2+, dysprosium ion Dy3+
Compound be raw material, by chemical formula Sr2MgSi2O7:xEu2+yDy3+zLi+Mol ratio weigh each raw material, 0.005≤x
≤ 0.03,0.01≤y≤0.05,0.015≤z≤0.03, grind and are well mixed；
(2) by the well mixed powder obtained in step (1), sintering time is 2~5 hours under weakly reducing atmosphere, sintering
Temperature is 1000 DEG C~1600 DEG C, adds activated carbon；
(3) powder sintered is cooled to room temperature and produces Li+The silicate fluorescent powder being co-doped with.
Further, above-mentioned Li+It is co-doped with silicate fluorescent material preparation method, described contains lithium ion Li+Compound
Selected from containing Li+Carbonate, hydroxide, nitrate, one kind in oxalates.Described contains magnesium ion M2-Compound is selected
From a kind of, the strontium ion Sr in MgO, MgCO32+Compound is SrCO3, silicon ion Si4+Compound is SiO2, europium ion Eu2+Change
Compound is Eu2O3, dysprosium ion Dy3+Compound be Dy2O3.5mol%~10mol% is added in the raw material of described step (1)
H3BO3Cosolvent mixed, followed by grinding.The sintering time of described step (2) is 2~3 hours, sintering
Temperature is 1100 DEG C~1500 DEG C.
Detailed description of the invention：
Li+ proposed by the present invention is co-doped with the method for improving silicate fluorescent powder long afterglow property, and its specific embodiment is such as
Under：
(1) according to Sr2MgSi2O7:xEu2+yDy3+zLi+(0.005≤x≤0.03、0.01≤y≤0.05、0.015≤z≤
0.03) stoichiometric proportion weighs raw material SrCO respectively3、SiO2、MgO、Li2CO3、Eu2O3And Dy2O3；
(2) 5mol%~10mol% H will be added in the raw material of step (1)3BO3Mixing is used as cosolvent；
(3) mixture obtained in step (2) is fully ground 4~5 hours in agate mortar；
(4) the well mixed powder obtained in step (3) is calcined 2~3 hours under weakly reducing atmosphere, calcining heat is
1100 DEG C~1500 DEG C, adding activated carbon will help to produce reducing atmosphere；
(5) powder calcined is cooled to room temperature, and by grinding diameter of particle control between 120~140 mesh；
The beneficial effect that the present invention is obtained：
1. it is co-doped with Li+When, more Lacking oxygens are generated, electronics is captured as trap, Sr can be effectively improved2MgSi2O7:
xEu2+,yDy3+The long afterglow property of fluorescent material.
2.Li+Fluxing agent can also be made, can effectively improve the crystallinity of crystal and expand the particle size of crystal,
So as to improve crystallization, long-persistence luminous intensity is finally improved.
3.Li+Charge compensation is made, makes trivalent Dy3+Replace divalence Sr2+When electric charge be compensated balance.
4th, the raw material that the present invention is used is cheap and easy to get, and production cost is low and is easy to industrialized production.
Embodiment
The present invention, but the protection domain being not intended to limit the invention will be expanded on further by specific embodiment below.
Those skilled in the art can be made improvements to preparation method and using instrument within the scope of the claims, and these improvement also should be regarded as
Protection scope of the present invention.
In following embodiments, unless otherwise indicated, described experimental method is generally built according to normal condition or manufacturer
The condition of view is implemented；Shown raw material, reagent can be obtained by way of commercially available purchase.
The present invention is used with H3BO3Li is synthesized for the high temperature solid-state method of cosolvent+The Sr being co-doped with2MgSi2O7:xEu2+,yDy3+
4 specific embodiments of fluorescent material are as shown in table 1.
The embodiment list of ingredients of table 1
Embodiment 1#(Sr1.955Li0.015Eu0.01Dy0.02MgSi2O7):
1 in composition such as table 1#Shown, specific preparation method comprises the following steps：
1. silicate solid powder stock SrCO is weighed respectively by the composition in table 13、SiO2、MgO、Li2CO3、Eu2O3With
Dy2O3Respectively 4.58g, 0.797g, 0.1805g, 0.0048g, 0.0685g and 0.1391g；
2. 200ml H will be added in step raw material 1.3BO3Mixing is used as cosolvent；
3. the mixture by step 2. middle acquisition is fully ground 4 hours in agate mortar；
4. the well mixed powder by step 3. middle acquisition is calcined 2 hours under weakly reducing atmosphere, and calcining heat is 1100
DEG C, adding activated carbon will help to produce reducing atmosphere；
5. the powder calcined is cooled to room temperature, and by grinding diameter of particle control in 120 mesh；
Test result is as follows：
Process 5. in sample after compressing tablet process carry out XRD tests, crystal structure is produced without significant change without attached phase.
SEM test displays are carried out, sample particle becomes large-sized, and boundary density diminishes, and without particle polymerization.Seen by the weak curve of sunset glow
Go out, as t=50s, SED-Li luminous intensities are 0.4cd/m2。
Embodiment 2#(Sr1.94Li0.02Eu0.02Dy0.02MgSi2O7):
2 in composition such as table 1#Shown, specific preparation method comprises the following steps：
1. silicate solid powder stock SrCO is weighed respectively by the composition in table 13、SiO2、MgO、Li2CO3、Eu2O3With
Dy2O3Respectively 8.2761g, 4.333g, 0.3181g, 0.01070g, 0.2425g and 0.2724g；
2. 220ml H will be added in step raw material 1.3BO3Mixing is used as cosolvent；
3. the mixture by step 2. middle acquisition is fully ground 4 hours in agate mortar；
4. the well mixed powder by step 3. middle acquisition is calcined 2 hours under weakly reducing atmosphere, and calcining heat is 1270
DEG C, adding activated carbon will help to produce reducing atmosphere；
5. the powder calcined is cooled to room temperature, and by grinding diameter of particle control in 130 mesh；
Test result is as follows：
Process 5. in sample after compressing tablet process carry out XRD tests, crystal structure is produced without significant change without attached phase.
SEM test displays are carried out, sample particle becomes large-sized, and boundary density diminishes, and without particle polymerization.Seen by the weak curve of sunset glow
Go out, as t=50s, SED-Li luminous intensities are 0.55cd/m2。
Embodiment 3#(Sr1.915Li0.025Eu0.01Dy0.05MgSi2O7)：
3 in composition such as table 1#Shown, specific preparation method comprises the following steps：
1. the composition pressed in table 1 weighs silicate solid powder stock SrCO3、SiO2、MgO、Li2CO3、Eu2O3And Dy2O3
Respectively 4.5708g, 2.4219g, 0.1778g, 0.00075g, 0.0677g and 0.3806g；
2. 240ml H will be added in step raw material 1.3BO3Mixing is used as cosolvent；
3. the mixture by step 2. middle acquisition is fully ground 5 hours in agate mortar；
4. the well mixed powder by step 3. middle acquisition is calcined 3 hours under weakly reducing atmosphere, and calcining heat is 1300
DEG C, adding activated carbon will help to produce reducing atmosphere；
5. the powder calcined is cooled to room temperature, and by grinding diameter of particle control in 140 mesh；
Test result is as follows：
Process 5. in sample after compressing tablet process carry out XRD tests, crystal structure is produced without significant change without attached phase.
SEM test displays are carried out, sample particle becomes large-sized, and boundary density diminishes, and without particle polymerization.Seen by the weak curve of sunset glow
Go out, as t=50s, SED-Li luminous intensities are 0.7cd/m2。
Embodiment 4#(Sr1.92Li0.03Eu0.03Dy0.02MgSi2O7)：
4 in composition such as table 1#Shown, specific preparation method comprises the following steps：
1. the composition pressed in table 1 weighs silicate solid powder stock SrCO3、SiO2、MgO、Li2CO3、Eu2O3And Dy2O3
Respectively 4.6105g, 2.4428g, 0.1793g, 0.00896g, 0.2051g and 0.1536g；
2. 250ml H will be added in step raw material 1.3BO3Mixing is used as cosolvent；
3. the mixture by step 2. middle acquisition is fully ground 5 hours in agate mortar；
4. the well mixed powder by step 3. middle acquisition is calcined 3 hours under weakly reducing atmosphere, and calcining heat is 1500
DEG C, adding activated carbon will help to produce reducing atmosphere；
5. the powder calcined is cooled to room temperature, and by grinding diameter of particle control in 140 mesh；
Process 5. in sample after compressing tablet process carry out XRD tests, crystal structure is produced without significant change without attached phase.
SEM test displays are carried out, sample particle becomes large-sized, and boundary density diminishes, and without particle polymerization.Seen by the weak curve of sunset glow
Go out, as t=50s, SED-Li luminous intensities are 0.58cd/m2。
Examples detailed above is the present invention preferably embodiment, but embodiments of the present invention are not limited by examples detailed above
System, other it is any without departing from spirit of the invention and the modification made under principle, modification, replacement, combine, simplification is equivalent
Substitute mode, be included within protection scope of the present invention.
Claims (7)
1. a kind of method for the long afterglow property for improving silicate fluorescent powder, it is characterised in that this method is by high silicic acid
Li is co-doped with salt+To improve silicate fluorescent powder long afterglow property, wherein, Li+It to be co-doped with by following formula the composition of silicate fluorescent powder
Show：
Sr2MgSi2O7:xEu2+yDy3+zLi+
The span of wherein x, y, z is respectively 0.005≤x≤0.03,0.01≤y≤0.05 and 0.015≤z≤0.03.
2. prepare a kind of Li as claimed in claim 1+It is co-doped with the method for silicate fluorescent powder, it is characterised in that this method includes
Following steps：
(1) to contain lithium ion Li+, magnesium ion M2-, strontium ion Sr2+, silicon ion Si4+, europium ion Eu2+, dysprosium ion Dy3+ change
Compound is raw material, by chemical formula Sr2MgSi2O7:xEu2+yDy3+zLi+Mol ratio weigh each raw material, 0.005≤x≤
0.03rd, 0.01≤y≤0.05,0.015≤z≤0.03, grind and are well mixed；
(2) by the well mixed powder obtained in step (1), sintering time is 2~5 hours, sintering temperature under weakly reducing atmosphere
For 1000 DEG C~1600 DEG C, activated carbon is added；
(3) powder sintered is cooled to room temperature, produces Li+The silicate fluorescent powder being co-doped with.
3. Li according to claim 2+It is co-doped with the preparation method of silicate fluorescent powder, it is characterised in that described contains lithium
Ion Li+Compound, which is selected from, contains Li+Carbonate, hydroxide, nitrate, one kind in oxalates.
4. Li according to claim 2+It is co-doped with the preparation method of silicate fluorescent powder, it is characterised in that described contains magnesium
Ion M2-A kind of, strontium ion Sr of the compound in MgO, MgCO32+Compound is SrCO3, silicon ion Si4+Compound is
SiO2, europium ion Eu2+Compound is Eu2O3, dysprosium ion Dy3+Compound be Dy2O3。
5. Li according to claim 2+It is co-doped with the preparation method of silicate fluorescent powder, it is characterised in that described step
(1) 5mol%~10mol% H is added in raw material3BO3Cosolvent mixed, followed by grinding.
6. Li according to claim 2+It is co-doped with the preparation method of silicate fluorescent powder, it is characterised in that described step
(2) sintering time is 2~3 hours, and sintering temperature is 1100 DEG C~1500 DEG C.
7. Li according to claim 2+It is co-doped with the preparation method of silicate fluorescent powder, it is characterised in that described step
(3) it is cooled to after room temperature, by grinding diameter of particle control between 120~140 mesh.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108715761A (en) * | 2018-07-06 | 2018-10-30 | 闽南师范大学 | A kind of strontium silicate zinc is the long afterglow luminescent powder and preparation method thereof of host material |
| CN114032090A (en) * | 2021-12-03 | 2022-02-11 | 广东电网有限责任公司 | Yellow-green afterglow material and preparation method thereof |
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| CN108715761B (en) * | 2018-07-06 | 2021-06-25 | 闽南师范大学 | Long-afterglow luminescent powder taking strontium zinc silicate as matrix material and preparation method thereof |
| CN114032090A (en) * | 2021-12-03 | 2022-02-11 | 广东电网有限责任公司 | Yellow-green afterglow material and preparation method thereof |
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