CN1594499A - Red long persistence luminescent materials and their synthesis process and use - Google Patents
Red long persistence luminescent materials and their synthesis process and use Download PDFInfo
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- CN1594499A CN1594499A CN 200410045034 CN200410045034A CN1594499A CN 1594499 A CN1594499 A CN 1594499A CN 200410045034 CN200410045034 CN 200410045034 CN 200410045034 A CN200410045034 A CN 200410045034A CN 1594499 A CN1594499 A CN 1594499A
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Abstract
The invention discloses a red long persistence luminescent materials, their synthesis process and use thereof, wherein the luminescent material employs alkaline earth metal titanate as substrate, Pr3++ as activator, other rare earth ions as co-activator, IIIA ions as sensitizing agent, and the preparing process consists of weighing by proportion, charging right amount of H3BO3, Pr(NO)3, NaNO, and one step synthesizing through high temperature solid phase reaction.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and relates to a luminescent material made of Pr3+Ions being activators, Mg2-m-n-kCamSrnBakZn4T15O36Is a substrateThe red long afterglow luminescent material and the synthesis method and the application thereof.
Background
Matsuzawa T reported SrAl2O4:Eu2+，Dy3+After the phenomenon of ultra-long afterglow, rare earth doped long afterglow materials arouse great interest. From the point of colorimetry, as long as the long-afterglow luminescent materials with three primary colors (red, green and blue) have stable chemical properties and similar afterglow intensity and decay time, the long-afterglow luminescent materials can be mixed according to a certain proportion to obtain the long-afterglow luminescent material with any color, otherwise the afterglow color of the mixed material changes in the decay process. The rare earth ion doped alkaline earth aluminate (silicate) green long afterglow and blue long afterglow luminescent material has entered into practical stage, and the green long afterglow luminescent material with best performance is known to be SrAl2O4:Eu2+，Dy3+The blue long afterglow material is SrAl2O4:Eu2+，Nd3+The chemical properties, afterglow intensity and decay time of the two longafterglow luminescent materials are similar. However, at present, no red long afterglow material with the performance matched with the performance exists.
The red long-afterglow luminescent materials which are found are divided into four main groups according to the matrix: alkaline earth metal sulfide system, sulfur oxide system, strontium aluminum composite sulfur oxide system, and alkaline earth metal titanate system. The first three systems of luminescent materials have good red long afterglow property, but the application is limited because the sulfur-containing material is easy to deteriorate in humid air and emit odor. Since the report of CaTiO3:Pr3+After having the characteristic of red long afterglow, Pr3+Activated alkaline earth metal titanates MTiO3The (M ═ Ca, Sr and Ba) red long afterglow luminescent material is a kind of red long afterglow luminescent material with stable performance, but the luminescent brightness and afterglow time do not reach the practical requirements.
CN1317537A describes a luminescent material capable of converting near ultraviolet light into blue light and red light and green light into red light. The luminescent material has both red long afterglow property and red and blue light emitting propertyIt is called single-base dual-energy light conversion agent. The single-base dual-energy light conversion agent is used for manufacturing an agricultural light conversion film, fully utilizes solar energy and develops photoecological agriculture. The invention relates to a single-base dual-energy light conversion agent described in CN1317537A, which is an alkaline earth metal sulfide luminescent material, and the invention adjusts matrix Mg1-m-n-kCamSrnBakThe type and content of the cation in S and the type and content of the activator ion regulate and control the excitation spectrum and the emission spectrum of the light conversion agent, so that the excitation spectrum and the emission spectrum are respectively matched with the reflection spectrum and the absorption spectrum of the plant. However, alkaline earth metal sulfides can cause deliquescence in air, and therefore, the use of such light conversion agents is limited.
Disclosure of Invention
The invention aims to solve the technical problem of providing an all-weather stable alkaline earth metal titanate red long afterglow luminescent material and a synthetic method and an application method thereof aiming at the defects in the prior art; the luminescent material has slow red long afterglow property, double-light property luminescent property of absorbing ultraviolet light to emit blue light and red light and absorbing green light to emit red light, and is a single-base double-energy light conversion agent which can be used for converting solar energy and promoting plant photosynthesis in agriculture.
The technical scheme adopted for solving the technical problem of the invention is that the general formula of the raw materials used by the red long afterglow luminescent material is as follows:
Mg2-m-n-kCamSrnBakZn4T15O36:xPr3+，yRE3+，zT3+，rR+
wherein: RE is one or two of La, Ce, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu,
t is one or two of B, Al, Ga, In, Ta and Bi.
R＝Li+，Na+，K+，Rb+，Cs+，Ag+One or two of them;
0≤m≤2.0，0≤n≤2.0，0≤k≤2.0，0≤m+n+k≤2.0
0＜x≤0.01，0≤y≤0.01，0≤z≤0.01，0＜r≤0.3
the maximum excitation wavelength is 320-380 nm and 440-590 nm, the maximum emission wavelength is 420-490 nm and 614nm and 640nm, and the red long afterglow luminescent material is an all-weather single-base dual-energy light conversion agent which can be used for light conversion agricultural films.
Mg2-m-n-kCamSrnBakZn4Ti15O36Pr has two significant properties: one is very slow red long afterglow, and the other is double-light emitting property of absorbing ultraviolet light to emit blue light and red light and absorbing green light to emit red light.
The invention has the following characteristics:
1. the invention relates to rare earth Pr3+Ion activated titanate red long afterglow luminescent material.
2. The red long-afterglow luminescent material features its chemical composition including alkaline-earth metal titanate as matrix and Pr3+As activators, other rare earth ions as co-activators, IIIAThe ion being a sensitizer, IAOr Ag+The ions are charge compensators.
3. The excitation spectrum of the red long-afterglow luminescent material is mainly characterized in that the ultraviolet region with the strongest excitation wavelength near 330nm and the green region with the wavelength near 560nm and 589nm can be excited by ultraviolet light and green light at the same time. The main characteristics of the emission spectrum are that the strongest emission wavelength is in a blue light region of 440-490 nm and red light regions of 612nm and 640 nm. I.e. blue and red light can be emitted simultaneously.
4. The red long-afterglow luminescent material can convert near ultraviolet light and green light in the spectrum of sunlight and artificial light source used in plant factories into blue light and red light effective for plant growth.
5. The red long-afterglow luminescent material can convert ultraviolet light with low photosynthesis efficiency in the solar spectrum and with 330nm as the center into blue light with 468nm as the center and red light with 612nm as the center. Green light with low photosynthesis efficiency and centered at 560nm is converted into red light with the centered at 612nm, and the light conversion agent is an all-weather sulfur-free single-base dual-energy light conversion agent.
6. The agricultural product made up by using all-weather sulfur-free single-base dual-energy light-converting agent and high-molecular resin is specially suitable for cultivating crops in low-temp. and low-light region, and can make crops mature earlier and optimize quality.
7. The luminescent material of the present invention may be also used in building material, industrial art and other fields to synthesize red luminous paint and other indicating material.
The synthesis method of the red long afterglow luminescent material comprises the following steps:
first, make up
The invention can adopt one of the following three methods to prepare the materials:
1. and (3) dry method:
① according to the reaction equation
② weighing Pr-containing compounds according to the formula6O11，RE2O3，R2CO3And T;
③ mixing all above materials, and grinding.
2. And (2) wet method:
① calculated (MgCO)3、CaCO3、SrCO3、BaCO3、ZnO2And TiO2Weighing, placing in an evaporation dish, and mixing;
② pipette Pr (NO)3, RE according to stoichiometric ratio3+，T3+And R+Adding nitrate solution or chloride solution of ions into the mixture in the ① evaporating dish, and stirring uniformly by a glass rod;
③ drying the raw material mixture in an oven, and grinding thoroughly.
3. Sol-gel method: adding citric acid into hexanediol liquid, dissolving with magnetic stirring, and adding Ti (OC) at a certain ratio4H9)4Magnetically stirring to obtain solution (I), Ca (NO)3)2、Zn(NO3)2、NaNO3、Pr(NO3)3Mixing into solution according to a certain proportion, heating to evaporate excessive water, concentrating to obtain solution (II), adding the solution II into the solution I dropwise under magnetic stirring to avoid Ti (OC)4H9)4Hydrolyzing, heating the mixture at 200 deg.C to make the solution color from light yellow → dark yellow → brown black → black glassy substance, heating the glassy substance at 400 deg.C for 2 hr, and grinding the product into powder in agate mortar. The method specifically comprises the following steps:
① citric acid is added to the hexanediol liquid in stoichiometric proportions, dissolved by magnetic stirring, and then a stoichiometric amount of Ti (OC) is added4H9)4And magnetically stirring to obtain solution (I).
② measuring Ca (NO) with pipette at a certain ratio3)2、Zn(NO3)2、NaNO3、Pr(NO3)3Mixing the solutions, heating in water bath to evaporate water, and concentrating to one third of the initial volume to obtain solution (II);
③ adding the solution II into the solution I drop by drop under magnetic stirring to obtain a mixed solution (III);
④ maintaining the mixed solution (III) at a constant temperature of 200 ℃ for 2-5 h to obtain a brownish black thick substance;
⑤ keeping the brown black paste at 400 deg.C for 1-2 h, cooling, and grinding into powder.
II, synthesis
The red long-afterglow luminescent material can be synthesized by one of the following two methods:
(1) high-temperature solid-phase synthesis: the synthesis temperature of the dry method and the wet method is 1200-1300 ℃, the burning time is 48-96 h, and the powder obtained by the sol-gel method is burned for 15-25 h at 700-1000 ℃ to obtain the required product. The specific method comprises the following steps: a crucible containing the ingredientsPlacing the crucible in a high temperature furnace, firing the mixture obtained by the dry method and the wet method at 1200-1300 ℃ for 4 g-96 h, firing the powder obtained by the sol-gel method at 700-1000 ℃ for 15-25 h to obtain the red long afterglow luminescent material Mg2-m-n-kCamSrnBakZn4T15O36:xPr3+，yRE3+，zT3+，rR+。
(2) Microwave radiation synthesis: heating for 1-2 h at 700-1000 ℃ to obtain the product. The specific method comprises the following steps: placing the crucible filled with the ingredients in a microwave oven, selecting microwave power, controlling the temperature to 700-1000 ℃, keeping heating for 30-120 min, and cooling to obtain the red long-afterglow luminescent material Mg2-m-n-kCamSrnBakZn4T15O36:xPr3+，yRE3+，zT3+，rR+。
Drawings
FIG. 1: excitation spectrum of red long afterglow luminescent material
FIG. 2: the emission spectrum of the red long afterglow luminescent material of the invention under the excitation of ultraviolet light
FIG. 3: the emission spectrum of the red long afterglow luminescent material of the invention under the excitation of green light
FIG. 4: emission spectrum of red long afterglow luminescent material
FIG. 5 shows the emission spectrum of the red long afterglow luminescent material of the present invention under the excitation of ultraviolet light
FIG. 6: the invention relates to a red long afterglow luminescent material Ca2Zn4Ti15O36Decay curve graph of afterglow of Pr
In the figure: lambda em-emission wavelength Lambda ex-excitation wavelength
Detailed Description
The following are non-limiting examples of the invention:
example 1: ca2Zn4Ti15O36Pr, Na (marked A)
The method comprises the following steps: according to CaCO3∶ZnO∶TiO20.8g of CaCO are weighed out in a molar ratio of 1: 2: 7.53，1.296gZnO，4.8gTiO2After fully grinding, adding 1.6X 10-5mol of Pr (NO)3)3Solution, 1.6X 10-5And drying the NaNO in mol, and filling the dried NaNO into a quartz crucible or a corundum crucible. Firing at 1200 ℃ for 48-96 h, cooling and grinding to obtain a sample;
the second method comprises the following steps: or loading the raw materials into small quartz crucible or corundum crucible, covering with a large quartz crucible or corundum crucible, filling Fe into the interlayer3O4And (3) placing the sample as a microwave absorbing medium in an industrial microwave oven of 2700W for burning for 1-2 h, gradually cooling, and grinding to obtain the sample.
The third method comprises the following steps: (1)0.472gCa (NO)3)2·4H2O+1.188g Zn(NO3)2·6H2O+0.2ml 2×10-5mol/ml Pr (NO)3)3Solution +0.2ml 2X 10-5NaNO in mol/ml3Heating to evaporate excessive water and concentrating; (2)5.1ml Ti (OC)4H9)4Dropwise adding a proper amount of hexanediol and citric acid solution, and magnetically stirring to obtain a transparent solution (II); (3) dropwise adding the solution I into the solution II under magnetic stirring to obtain a mixed solution (III), heating to 200 ℃ for 5 hours, heating to 400 ℃ for 2 hours, and grinding the obtained solid precursor into powder; (4) grinding the solid into powder, and firing the powder at 700-1000 ℃ for 15-25 h to obtain a target product.
The method four comprises the following steps: the first three steps are the same as the third steps (1) to (3), and the solid precursor obtained in the step (4) is placed in an industrial microwave oven of 2700W for burning for 1-2 hours to obtain a target product.
(A) Characteristic excitation and emission spectra of (a) are shown in fig. 1, 2 and 3.
Example 2: ca2Zn4Ti15O36Pr, Al (marked as B)
Weighing CaCO according to stoichiometric ratio30.8g，ZnO 1.296g，TiO24.8g，0.0936gAl(OH)3. Adding 1.6X 10-5mol of Pr (NO)3、1.6×10-5mol of NaNO3Mixing with proper amount of ethanol, naturally drying, loading into a quartz crucible or a corundum crucible, and burning at 1200 ℃ for 48-96 h. And gradually cooling to obtain the sample.
Doped with Al3+The luminous intensity of the product was significantly improved, and fig. 4 is a comparison of the red emission intensity of (a) (B).
Example 3: ca1.5Sr0.5Zn4Ti15O36Pr, Na (marked C)
According to CaCO3∶SrCO3∶ZnO∶TiO20.6g of CaCO was weighed in a molar ratio of 1.5: 0.5: 4: 153，0.269gSrCO3，1.296gZnO，4.8gTiO2After fully grinding, adding 1.6X 10-5mol of Pr (NO)3，1.6×10-5mol of NaNO3And drying and transferring into a quartz crucible or a corundum crucible. Firing at 1200 ℃ for 48-96 h, cooling and grinding to obtain the sample.
Example 4: ca1.5Ba0.5Zn4Ti15O36Pr, Na (marked as D)
According to CaCO3∶BaO∶ZnO∶TiO20.45g of CaCO was weighed in a molar ratio of 1.5: 0.5: 4: 153，0.2295gBaO，0.972gZnO，3.6gTiO2After fully grinding, adding 1.6X 10-5mol of Pr (NO)3，1.6×10-5mol of NaNO3And drying and then loading into a quartz crucible or a corundum crucible. Firing at 1200 ℃ for 48-96 h, cooling and grinding to obtain the sample.
Example 5: ca2Zn4Ti15O36Pr, Gd, Na (marked as E)
Weighing CaCO according to stoichiometric ratio30.8g，ZnO1.296g，TiO24.8g，1.6×10-5mol of Pr (NO)3，0.8×10-5mol Gd(NO3)3，1.6×10-5mol of NaNO3. After being evenly ground, the mixture is put into a quartz crucible or a corundum crucible and is burnt for 48 to 96 hours at 1200 ℃. And gradually cooling to obtain the sample.
The application of the red long afterglow luminescent material of the invention is as follows:
can be used for melting with plastic raw materials to prepare agricultural plastic product master batches with various functions.
Can be used as an all-weather sulfur-free single-base dual-energy light conversion agent: the double-energy light conversion rare earth master batch (I) is prepared by the following steps:
the ingredients of the feed can be as follows: 96Kg of polyethylene and 4Kg of dual-energy light conversion agent of the red long-afterglow luminescent material of the invention are mixed, dispersed, melted and extruded into granules, thus obtaining the dual-energy light conversion master batch.
The double-energy light conversion rare earth antifogging master batch (II) is prepared by the following steps:
the ingredients of the feed can be as follows: 86Kg of polyethylene, 4Kg of dual-energy light conversion agent of the red long afterglow luminescent material of the invention and 4Kg of dehazing agent FY-1 or FY-210 Kg of the red long afterglow luminescent material of the invention are mixed, dispersed, melted and extruded into particles, thus obtaining the dual-energy light conversion antifogging master batch.
The double-energy light conversion rare earth multifunctional master batch (III) with the functions of light conversion, fog prevention and heat preservation is prepared by the following steps:
the ingredients of the feed can be as follows: 46Kg of polyethylene, 4Kg of dual-energy light conversion agent of red long afterglow luminescent material, 10Kg of dripping agent, 4Kg of dehazing agent FY-1 or FY-210 Kg of light stabilizer Chmmassorb944LD 5Kg of heat insulating agent CaCO325Kg, mixing, dispersing, melting, extruding and granulating to obtain the multifunctional master batch. The multifunctional master batch has the functions of light conversion, fog prevention and heat preservation.
Can be used for preparing agricultural plastic products with various functions: the double-energy light conversion rare earth master batch is added into high molecular resin according to 0.1-1.0% of the effective concentration of a light conversion agent and is applied to synthesizing light conversion agricultural films, agricultural greenhouse light conversion plates and other materials applied to plant cultivation.
The all-weather (sulfur-free) single-base dual-energy light conversion agent can be used as a light functional additive to be directly sprayed on plants.
Claims (9)
1. A red long-afterglow luminescent material is prepared from alkaline-earth metal titanate as matrix and rare-earth ions Pr3+The ions being activatorsThe other metal ions are sensitizing agents, and the composition general formula of the sensitizing agents is as follows:
Mg2-m-n-kCamSrnBakZn4T15O36：xPr3+，yRE3+，zT3+，rR+wherein: RE is one or two of La, Ce, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu;
one or two of T ═ B, Al, Ga, In, Ta and Bi;
R＝Li+，Na+，K+，Rb+，Cs+，Ag+one or two of them; m is more than or equal to 0 and less than or equal to 2.0, n is more than or equal to 0 and less than or equal to 2.0, k is more than or equal to 0 and less than or equal to 2.0, and m + n + k is more than or equal to 0 and less than or equal to 2.0; x is more than 0 and less than or equal to 0.01, y is more than or equal to 0 and less than or equal to 0.01, z is more than 0 and less than or equal to 0.01, r is more than 0 and less than or equal to 0.3, the maximum excitation wavelength is 320-380 nm and 440-590 nm, the maximum emission wavelength is in the regions of 420-490 nm, 614nm and 640nm, and the red long-afterglow luminescent material is an all-weather sulfur-free single-base dual-energy light conversion agent which can be used for light conversion agricultural films.
2. A method for synthesizing the red long-afterglow luminescent material of claim 1, which is characterized by comprising the steps of:
preparing materials: the ingredients can be prepared by one of the following three methods:
(1) and (3) dry-method material preparation: calculating the weight of the raw materials according to the metering ratio of each element in the general formula; namely, according to the reaction equation:
mixing the above materials uniformly for use
(2) And (3) wet-process batching: calculating the weight of the raw materials according to the metering ratio of each element in the general formula; namely, according to the reaction equation:
fully grinding the raw materials in bowl, adding proper quantity of ethyl alcohol, uniformly mixing them and naturally drying for stand-by
(3) Sol-gel method: adding citric acid into hexanediol liquid, magnetically stirring to dissolve, and dissolvingAdding Ti (OC) in a stoichiometric ratio4H9)4Magnetically stirring to obtain solution (I), Ca (NO)3)2、Zn(NO3)2、NaNO3、Pr(NO3)3Mixing into solution according to a certain proportion, heating to evaporate excessive water, concentrating to obtain solution (II), adding the solution II into the solution I dropwise under magnetic stirring to avoid Ti (OC)4H9)4Hydrolyzing, heating the mixture at 200 deg.C to make the solution color from light yellow → dark yellow → brown black → black glassy substance, heating the glassy substance at 400 deg.C for 2 hr, grinding the product into powder in agate mortar,
synthesizing: after the materials are mixed, the red long afterglow luminescent material can be synthesized by one of the following two methods:
(1) high-temperature solid-phase synthesis: the synthesis temperature of the dry method and the wet method is 1200-1300 ℃, the burning time is 48-96 h, the powder obtained by the sol-gel method is burned for 15-25 h at 700-1000 ℃ to obtain the required product,
(2) microwave synthesis: heating for 1-2 h at 700-1000 ℃ to obtain the product.
3. The method for synthesizing the red long-afterglow luminescent material of claim 1 as claimed in claim 2, wherein MCO is adopted3(M＝Mg，Ca，Sr，Ba)∶ZnO∶TiO2Accurately weighing the substances according to the weight ratio of 1: 2: 7.5, and adding a proper amount of Pr (NO)3NaNO, and carrying out high-temperature 1200-1300 solid-phase reaction one-step synthesis.
4. The application of the red long-afterglow luminescent material as defined in claim 1 may be used in smelting plastic material to produce various functional mother material for agricultural plastic product.
5. The application of the red long-afterglow luminescent material as claimed in claim 4, wherein the following raw materials are used for preparing the dual-energy light-converting rare earth master batch (I): 96Kg of polyethylene and 4Kg of dual-energy light conversion agent of red long afterglow luminescent material are mixed, dispersed, melted and extruded into granules, thus obtaining the dual-energy light conversion master batch.
6. The application of the red long-afterglow luminescent material as claimed in claim 4, wherein the double-energy light-conversion rare earth anti-fog master batch (II) can be prepared from the following raw materials in proportion: 86Kg of polyethylene, 4Kg of dual-energy light conversion agent of red long afterglow luminescent material and 4Kg of dehazing agent FY-1 or FY-210 Kg of the mixture are mixed, dispersed, melted and extruded into particles to obtain the dual-energy light conversion antifogging master batch.
7. The application of the red long-afterglow luminescent material as claimed in claim 4,wherein the raw materials are used to prepare a dual-energy light-conversion rare earth multifunctional master batch (III) with light conversion, antifogging and heat preservation functions: 46Kg of polyethylene, 4Kg of dual-energy light conversion agent for red long-afterglow luminescent materials, 10Kg of drip agent, 944LD 5Kg of light stabilizer Chmmassorb and CaCO as heat-insulating agent3And 25Kg, mixing, dispersing, melting and extruding into granules to obtain the multifunctional master batch with the functions of light conversion, fog prevention and heat preservation.
8. The application of the red long-afterglow luminescent material as claimed in claim 4, 5, 6 or 7, which can be used for preparing agricultural plastic products with various functions: the double-energy light conversion rare earth master batch is added into high molecular resin according to 0.1-1.0% of the effective concentration of a light conversion agent and is applied to synthesizing light conversion agricultural films, agricultural greenhouse light conversion plates and other materials applied to plant cultivation.
9. The use of the red long-lasting phosphor according to claim 1, wherein the red long-lasting phosphor can be directly applied to plants as a light functional adjuvant.
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| CN103194227A (en) * | 2013-04-01 | 2013-07-10 | 潍坊大耀新材料有限公司 | Method for preparing red long-afterglow luminescent powder |
| CN103215041A (en) * | 2013-05-17 | 2013-07-24 | 南开大学 | Preparation method of near infrared super-long afterglow luminescence nanomaterial |
| CN103215041B (en) * | 2013-05-17 | 2014-11-19 | 南开大学 | Preparation method of near infrared super-long afterglow luminescence nanomaterial |
| CN104830331A (en) * | 2015-05-21 | 2015-08-12 | 湖南师范大学 | Complex phase red long afterglow phosphor and preparation method thereof |
| CN114456808A (en) * | 2022-02-22 | 2022-05-10 | 同济大学 | Tantalate-based red long-afterglow luminescent material and preparation method thereof |
| WO2023221150A1 (en) * | 2022-05-18 | 2023-11-23 | 五邑大学 | Fluorescence temperature measurement material, and preparation method therefor and application thereof |
| CN116179006A (en) * | 2022-12-30 | 2023-05-30 | 中国科学院福建物质结构研究所 | Long-afterglow luminous paint, preparation method and application thereof |
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