CN107189776B - Green silicate long-afterglow luminescent material and preparation method thereof - Google Patents
Green silicate long-afterglow luminescent material and preparation method thereof Download PDFInfo
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Abstract
A green silicate long-afterglow luminescent material and its preparation method, the chemical expression of the luminescent material is K2Ba7‑x‑ ySi16O40:xEu2+,yRIII(ii) a Wherein x is more than or equal to 0.001 and less than or equal to 0.5, and y is more than or equal to 0 and less than or equal to 0.5. By containing potassium ion K+Barium ion Ba2+Silicon ion Si4+Rare earth ion Eu2+And RIIIIs taken as a raw material and is expressed by a chemical expression K2Ba7‑x‑ySi16O40:xEu2+,yRIIIWeighing raw materials according to the stoichiometric ratio of the elements, grinding and uniformly mixing to obtain raw material powder; calcining under a reducing atmosphere; cooling to room temperature along with the furnace to obtain a calcined substance; grinding to obtain the green silicate long-afterglow luminescent material. The luminescent material has good chemical stability and thermal stability, is stable when meeting water, has simple preparation method, does not discharge waste water and waste gas, and can continuously emit the long-afterglow luminescent material with green afterglow.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, relates to a long-afterglow luminescent material, and particularly relates to a silicate long-afterglow luminescent material capable of emitting continuous visible green afterglow after being irradiated by ultraviolet light or visible light; the invention also relates to a preparation method of the luminescent material.
Background
The long-afterglow luminescent material belongs to one kind of photoluminescence material, which generates light under the condition of excitation of an external light source, absorbs light energy at the same time, stores the light energy, and slowly releases the stored energy in the form of light after the excitation is stopped. Regarding the system of the long afterglow material, the early traditional long afterglow material mainly focuses on the sulfide system such as ZnS, CaS and the like, and the system has the advantages of rich luminescent color and capability of covering a luminescent region from blue to red, but has the defects of poor stability, easy decomposition in air, low initial afterglow brightness, short afterglow time and the like. Subsequently, aluminate systems were extensively studied and developed, among which SrAl2O4:Eu2+,Dy3+Its advantages are high afterglow brightness, long afterglow time and high chemical stability, but poor water resistance and less luminescent colour. Aiming at the defects, the silicon has good chemical stability, a plurality of luminescent colors, rich and cheap raw material sourcesThe acid salt system has become a hot spot for the development of long afterglow materials in recent years. The patent "a long afterglow silicate long afterglow luminescent material and its preparation method" (patent No. CN201010516567.6, publication No. CN101974324A, publication No. 2011.02.16) discloses a silicate long afterglow luminescent material and its preparation method, said luminescent material chemical composition is Ba3.992-xSi6O16:Eu0.008,RxWherein, R is one or two of Nd, Dy, Tm, La, Y, Pr, Tb or Ho, x is more than or equal to 0.005 and less than or equal to 0.050, and the material has blue-green light afterglow of more than 10 h. Patent "a silicate long afterglow phosphor and its preparation method" (patent No. CN201110411788.1, publication No. CN102433121A, published Japanese 2012.05.02) discloses a silicate long afterglow phosphor, the component of which is Na5Y1-xRExZrSi6O18Wherein RE is at least one of La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu trivalent rare earth, x is the molar percentage coefficient of doping of at least one of rare earth ions RE, x is more than or equal to 0 and less than or equal to 1.0, and the material has cyan afterglow of more than 2 hours. But the afterglow luminous intensity and the persistence time of the silicate long afterglow phosphor are still to be improved compared with those of aluminate long afterglow phosphor.
Disclosure of Invention
The invention aims to provide a green silicate long-afterglow luminescent material with wide excitation spectrum range and long afterglow time aiming at the problems of the silicate long-afterglow luminescent material.
The invention also aims to provide a preparation method of the green silicate long-afterglow luminescent material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a long-afterglow green silicate luminescent material with chemical expression K2Ba7-x-ySi16O40: xEu2+, yRIII(ii) a Wherein x is more than or equal to 0.001 and less than or equal to 0.5, and y is more than or equal to 0 and less than or equal to 0.5; rIII=Tb3+、Ce3+、Dy3+、Tm3+、Nd3+、Gd3+、Y3+、Er3+、La3+、Pr3+、Sm3+、Yb3+、Lu3+、Ho3+One or two of them.
The other technical scheme adopted by the invention is as follows: the preparation method of the green silicate long-afterglow luminescent material comprises the following steps:
step 1: by containing potassium ion K+Barium ion Ba2+Silicon ion Si4+Rare earth ion Eu2+And RIIIIs taken as a raw material and is expressed by a chemical expression K2Ba7-x-ySi16O40: xEu2+, yRIIIWeighing raw materials according to the stoichiometric ratio of the elements, wherein in the chemical expression, RIIIIs rare earth ion Tb3+、Ce3+、Dy3+、Tm3+、Nd3+、Gd3+、Y3+、Er3+、La3+、Pr3+、Sm3+、Yb3+、Lu3+、Ho3+One or two of them are selected from the group,
grinding and uniformly mixing the raw material powder to obtain raw material powder;
step 2: placing the raw material powder prepared in the step 1 in an environment with the temperature of 1050-1250 ℃, and calcining for 3-6 hours in a reducing atmosphere;
and step 3: cooling the calcined raw material powder to room temperature along with the furnace to obtain a calcined substance;
and 4, step 4: and (4) grinding the calcined substance obtained in the step (3) to prepare the long-afterglow luminescent material.
The long-afterglow luminescent material of green silicate of the invention takes silicate as a substrate, has good chemical stability and thermal stability, is stable when meeting water, has simple preparation method, does not discharge waste water and waste gas, and can continuously emit green afterglow after being excited by light with wavelength of 250 nm-500 nm.
Drawings
FIG. 1 is an XRD spectrum of a long-lasting phosphor prepared in example 1.
FIG. 2 is the excitation and emission spectra of the long persistence luminescent material prepared in example 1.
FIG. 3 is a graph showing the decay of afterglow of the long afterglow luminescent material obtained in example 1.
FIG. 4 is a thermoluminescence spectrum of the long-afterglow luminescent material obtained in example 1.
FIG. 5 is a thermoluminescence spectrum of the long-afterglow luminescent material obtained in example 2.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The chemical expression of the green silicate long afterglow luminescent material is K2Ba7-x-ySi16O40: xEu2+,yRIII(ii) a Wherein x is more than or equal to 0.001 and less than or equal to 0.5, and y is more than or equal to 0 and less than or equal to 0.5; rIIIIs Tb3+、Ce3+、Dy3+、Tm3+、Nd3+、Gd3+、Y3+、Er3+、La3+、Pr3+、Sm3+、Yb3+、Lu3+、Ho3+One or two of them.
The preparation method of the green silicate long-afterglow luminescent material specifically comprises the following steps:
step 1: by containing potassium ion K+Barium ion Ba2+Silicon ion Si4+Rare earth ion Eu2+And RIIIIs taken as a raw material and is expressed by a chemical expression K2Ba7-x-ySi16O40: xEu2+, yRIIIWeighing raw materials according to the stoichiometric ratio of the elements, wherein in the chemical expression, RIIIIs rare earth ion Tb3+、Ce3+、Dy3+、Tm3+、Nd3+、Gd3+、Y3+、Er3+、La3+、Pr3+、Sm3+、Yb3+、Lu3+、Ho3+One or two of them are selected from the group,
grinding and uniformly mixing the raw material powder;
step 2: placing the raw material powder obtained in the step 1 in an environment with the temperature of 1050-1250 ℃, and calcining for 3-6 hours in a reducing atmosphere;
the reducing atmosphere can employ three gases: the first is ammonia (NH)3) (ii) a The second is hydrogen (H) with the volume percentage of 5-25 percent2) And 95-75% nitrogen (N)2) A mixed gas of the components; the third is composed of 5-25% carbon monoxide (CO) and 95-75% nitrogen (N) by volume percentage2) A mixed gas of the components;
and step 3: cooling the calcined raw material powder to room temperature along with the furnace to obtain a calcined substance;
and 4, step 4: and (4) grinding the calcined substance obtained in the step (3) to obtain the green silicate long-afterglow luminescent material.
K2Ba7Si16O40: Eu2+Is a new luminescent material, has green light emission with peak value at 500mn under blue light excitation, and Nd is added into the material3+、Ho3+The trivalent rare earth ion coactivator can effectively adjust the distribution of traps in the material. Structurally, it is due to the matrix material K2Ba7Si16O40The rare earth metal complex has various cation lattices, and trivalent rare earth ions can generate more defects by non-equivalent substitution, thereby being beneficial to generating afterglow. After the ultraviolet light irradiation, the excitation source is removed, and bright green afterglow can be observed by human eyes and the duration time exceeds 10 hours.
Example 1
According to K2Ba6.98Si16O40：0.01Eu2+, 0.01Ho3+The stoichiometric ratio shown in the molecular formula is 0.0691gK2CO3、0.6887g BaCO3、0.4807g SiO2、0.0009g Eu2O3And 0.0009g Ho2O3Grinding and uniformly mixing the weighed raw materials as raw materials, putting the raw materials into an alumina crucible, calcining the raw materials for 3 hours in a reducing atmosphere at the temperature of 1250 ℃, wherein the reducing atmosphere consists of 95 percent of nitrogen and 5 percent of hydrogen in percentage by volume, and cooling calcined raw material powder to room temperature along with a furnace to obtain a calcined substance; and grinding to obtain the luminescent material. FIG. 1 shows an XRD spectrum of the luminescent material, which shows thatPhase K2Ba7Si16O40. The excitation and emission spectrum of the luminescent material is shown in FIG. 2, which shows that the emission spectrum of the long afterglow luminescent material is broadband emission, the peak value is near 500nm, and the emission spectrum is classified as Eu2+4f of65d1→4f7Transition, the strongest peak of the excitation spectrum is located at 365 nm. The color coordinates of the light emitted by the luminescent material calculated by using the CIE chromaticity diagram are x =0.25, y =0.45, and are located in the green emission region, which indicates that the luminescent material prepared in example 1 is a green luminescent material. FIG. 3 is the afterglow decay curve diagram of the luminescent material, and it can be seen from the graph that the luminescent material can continuously emit light with the duration of 10h, which can be distinguished by human eyes, and the luminous brightness is 0.32mcd/m2The above visible light indicates that the luminescent material is a long-afterglow luminescent material. FIG. 4 shows sample K at 0.0010g2Ba6.98Si16O40：0.01Eu2+, 0.01Ho3+And (3) measuring the pyroelectric spectrum after a light source with the wavelength of 254nm and a light source with the wavelength of 365nm are simultaneously irradiated for 5 min. It can be seen that a strong heat release peak suitable for long afterglow at room temperature exists in the sample at the temperature of 25-100 ℃, and the peak value is located near 47 ℃.
Example 2
According to K2Ba6.99Si16O40：0.005Eu2+, 0.005Nd3+The stoichiometric ratio shown in the molecular formula is 0.0691gK2CO3、0.6897g BaCO3、0.4807g SiO2、0.0004g Eu2O3And 0.0005g Nd2O3Grinding and uniformly mixing the weighed raw materials as raw materials, putting the raw materials into an alumina crucible, calcining the raw materials for 5 hours in a reducing atmosphere at the temperature of 1150 ℃, wherein the reducing atmosphere consists of 75% of nitrogen and 25% of hydrogen in percentage by volume, and cooling calcined raw material powder to room temperature along with a furnace to obtain a calcined substance; grinding to obtain the green silicate long-afterglow luminescent material. FIG. 5 shows sample K at 0.0010g2Ba6.99Si16O40：0.005Eu2+, 0.005Nd3+And (3) measuring the pyroelectric spectrum after a light source with the wavelength of 254nm and a light source with the wavelength of 365nm are simultaneously irradiated for 2 min. It can be seen thatThe sample has a heat release peak with a peak value near 65 ℃ in the temperature range of 25-150 ℃. It can be seen that Nd is co-doped3+Generates a relative Ho3+Deeper traps extend the persistence duration.
Example 3
According to K2Ba6.98Si16O40：0.01Eu2+, 0.01Dy3+The stoichiometric ratio shown in the molecular formula is 0.0691gK2CO3、0.6887g BaCO3、0.4807g SiO2、0.0009g Eu2O3And 0.0009g Dy2O3Grinding and uniformly mixing the weighed raw materials, putting the raw materials into an alumina crucible, placing the alumina crucible in an environment with the temperature of 1050 ℃, calcining for 6 hours in a reducing atmosphere, wherein the reducing atmosphere consists of 85% of nitrogen and 15% of hydrogen according to volume percentage, and cooling calcined raw material powder to room temperature along with a furnace to obtain a calcined substance; grinding to obtain the green silicate long-afterglow luminescent material.
Example 4
According to K2Ba6.98Si16O40：0.001Eu2+, 0.001Tm3+The stoichiometric ratio of the molecular formula is 0.0691gK2CO3、0.6887g BaCO3、0.4807g SiO2、0.0009g Eu2O3And 0.0009g Tm2O3Grinding and uniformly mixing the weighed raw materials, putting the mixture into an alumina crucible, placing the alumina crucible in an environment with the temperature of 1100 ℃, calcining for 5.5 hours in a reducing atmosphere, wherein the reducing atmosphere is ammonia gas, and cooling calcined raw material powder to room temperature along with a furnace to obtain a calcined substance; grinding to obtain the green silicate long-afterglow luminescent material.
Example 5
According to K2Ba6.98Si16O40：0.01Eu2+,0.005Ho3+, 0.005Nd3+The stoichiometric ratio of the molecular formula is 0.0691g K2CO3、0.6887g BaCO3、0.4807g SiO2、0.0009g Eu2O3、0.0005g Ho2O3、0.0005gNd2O3Grinding and uniformly mixing the weighed raw materials, putting the raw materials into an alumina crucible, placing the alumina crucible in an environment with the temperature of 1200 ℃, calcining for 3.5 hours in a reducing atmosphere, wherein the reducing atmosphere consists of 5 percent of carbon monoxide and 95 percent of nitrogen according to volume percentage, and cooling calcined raw material powder to room temperature along with a furnace to obtain a calcined substance; grinding to obtain the green silicate long-afterglow luminescent material.
Example 6
According to K2Ba6.99Si16O40：0.01Eu2+The stoichiometric ratio of the molecular formula is 0.0691g K2CO3、0.6897gBaCO3、0.4807g SiO2、0.0009g Eu2O3Grinding and uniformly mixing the weighed raw materials, putting the mixture into an alumina crucible, putting the alumina crucible into an environment with the temperature of 1200 ℃, calcining for 3.5 hours in a reducing atmosphere, wherein the reducing atmosphere consists of 25 percent of carbon monoxide and 75 percent of nitrogen according to volume percentage, and cooling calcined raw material powder to room temperature along with a furnace to obtain a calcined substance; grinding to obtain the green silicate long-afterglow luminescent material.
Example 7
According to K2Ba6.99Si16O40：0.5Eu2+,0.2Sm3+,0.3Yb3+Stoichiometric ratio of formula, taking K2CO3、BaCO3、SiO2、Eu2O3、Sm2O3And Yb2O3Grinding and uniformly mixing the weighed raw materials, putting the mixture into an alumina crucible, placing the alumina crucible in an environment with the temperature of 1150 ℃, calcining for 4.5 hours in a reducing atmosphere, wherein the reducing atmosphere consists of 15% of carbon monoxide and 85% of nitrogen according to volume percentage, and cooling calcined raw material powder to room temperature along with a furnace to obtain a calcined substance; grinding to obtain the green silicate long-afterglow luminescent material.
Claims (2)
1. A green silicate long-afterglow luminescent material is characterized by that it has a K-value2Ba6.98Si16O40：0.01Eu2+, 0.01Ho3+The stoichiometric ratio of the formula (I) is,weigh 0.0691g K2CO3、0.6887g BaCO3、0.4807g SiO2、0.0009gEu2O3And 0.0009g Ho2O3Grinding and uniformly mixing the weighed raw materials as raw materials, putting the raw materials into an alumina crucible, calcining the raw materials for 3 hours in a reducing atmosphere at the temperature of 1250 ℃, wherein the reducing atmosphere consists of 95 percent of nitrogen and 5 percent of hydrogen in percentage by volume, and cooling calcined raw material powder to room temperature along with a furnace to obtain a calcined substance; and grinding to obtain the luminescent material.
2. A green silicate long-afterglow luminescent material is characterized by that it has a K-value2Ba6.99Si16O40：0.005Eu2+,0.005Nd3+In the stoichiometric ratio shown in the formula, 0.0691g K is weighed2CO3、0.6897g BaCO3、0.4807g SiO2、0.0004g Eu2O3And 0.0005g Nd2O3Grinding and uniformly mixing the weighed raw materials as raw materials, putting the raw materials into an alumina crucible, calcining the raw materials for 5 hours in a reducing atmosphere at the temperature of 1150 ℃, wherein the reducing atmosphere consists of 75% of nitrogen and 25% of hydrogen in percentage by volume, and cooling calcined raw material powder to room temperature along with a furnace to obtain a calcined substance; grinding to obtain the green silicate long-afterglow luminescent material.
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