CN113265252A - Preparation method of white fluorescent powder and magnesium tantalate - Google Patents
Preparation method of white fluorescent powder and magnesium tantalate Download PDFInfo
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Abstract
The invention discloses a preparation method of white light fluorescent powder, which comprises the following steps: mixing and tabletting raw materials required for synthesis; placing the pressed body in a reducing atmosphere, and reacting for 8-12h at the temperature of 1400 ℃ and 1600 ℃; crushing the cooled pressed sheet to obtain the fluorescent powder, wherein the chemical structural formula of the fluorescent powder is Mg4Ta2‑ xO9：TbxAnd X is more than or equal to 0.001 and less than or equal to 0.006, the scheme prepares the fluorescent powder by a solid phase method, the fluorescent powder is obtained by tabletting, reacting and crushing, the synthetic atmosphere is subjected to micro-regulation and control in the reaction process, and the fluorescent powder is synthesized in a reducing atmosphere.
Description
Technical Field
The invention relates to the technical field of fluorescent powder materials, in particular to a preparation method of white fluorescent powder with pure luminescence, a preparation method of magnesium tantalate and a solid-phase synthesis method for preparing the magnesium tantalate.
Background
White Light Emitting Diodes (WLEDs) are a new type of solid state lighting device, which has, compared to other light sources: the LED light source has the advantages of small size, solidification, vibration resistance, difficult damage, energy conservation, high light efficiency, long service life, no pollution, instant start, no stroboflash and the like, and is expected to become the most important light source in the future.
At present, the preparation method mainly comprises two methods: one is composed of an InGaN blue LED chip with the emission wavelength of 460nm and YAG: the blue light emitted by the chip excites the fluorescent powder to emit yellow light, and the blue light and the yellow light are mixed to obtain white light, but the red light emitting component is insufficient, and the white light emitting performance is unstable.
The second scheme is to use an ultraviolet-near ultraviolet chip to excite a tricolor phosphor (RGB mixed phosphor) to realize white light emission, for example, in a document with the patent application number CN2019105169235, phosphors of various colors such as blue, cyan, green, red and the like are mixed to pursue the effect of warm white light, but obviously, the problems of complex forming process, difficult proportion regulation and control and serious self-absorption phenomenon can be seen.
In contrast, a scheme of emitting white light by using single-matrix fluorescent powder appears in the market, but the color coordinates of most of the disclosed schemes are far away from the color coordinates (0.33 ) of pure white light, and the luminous effect cannot meet the requirement.
Therefore, the single-matrix fluorescent powder is improved to further improve the white light effect.
Disclosure of Invention
In order to solve at least one technical defect, the invention provides the following technical scheme:
the application document discloses a preparation method of white light fluorescent powder, which comprises the following steps:
mixing and tabletting raw materials required for synthesis;
placing the pressed body in a reducing atmosphere, and reacting for 8-12h at the temperature of 1400 ℃ and 1600 ℃;
crushing the cooled pressed sheet to obtain the fluorescent powder, wherein the chemical structural formula of the fluorescent powder is Mg4Ta2-xO9：Tbx，0.001≤X≤0.006。
The magnesium tantalate is a single-matrix fluorescent powder, belongs to a hexagonal corundum structure, has an emission wavelength within a visible light range of 380 plus 800nm, has emission peaks mainly at 365nm, 460nm and 680nm, and has a white light color coordinate close to a pure white light color coordinate formed by two luminescence peaks at 460nm and 680 nm.
According to the scheme, the fluorescent powder is prepared by a solid-phase method, the fluorescent powder is obtained by tabletting, reacting and crushing, the synthetic atmosphere is subjected to micro control in the reaction process, and is synthesized in a reducing atmosphere, detection shows that the synthesis process is helpful for the fluorescent powder to enhance the luminescence of 460nm and weaken the luminescence of 365nm, and then Tb (terbium) ions are doped to enhance the green light part of magnesium tantalate, so that the white light obtained by tests is closer to the color coordinate of pure white light, and the fluorescent powder has good controllability.
The whole preparation process is short, the operation is easy, the raw material selection range is wide, the controllability is strong, the large-scale production is easy to realize, and the prepared fluorescent powder has good luminous effect and high yield.
Wherein, the value of X can be selected from the range of 0.001-0.002, 0.001-003, 0.002-0.004, 0.003-0.006,0.001-0.004, etc., specifically 0.001, 0.002, 0.003, 0.004, 0.005, 0.006, 0.0015, 0.0026, 0.0037, 0.0042, 0.0051, etc.
In the preparation method, alternative raw material forms are as follows: the raw materials comprise oxides or compounds of elements in a chemical formula, such as salts, preferably, the raw materials are oxides of tantalum, oxides of terbium and magnesium oxide or magnesium salts, and specifically: the raw material is Ta2O5、Tb4O7And MgO.
The preferred raw material ratio is: the MgO and Ta2O5In a molar ratio of 4 to 4.08, Tb4O7And Ta2O5The molar ratio of (A) is 0.00025-0.0015. MgO and Ta are preferable2O5The molar ratio of (A) is 4-4.04, or 4-4.05, or 4-4.03, or 4-4.02, etc. Preferably Tb4O7And Ta2O5The molar ratio of (A) is 0.00025-0.0005, 0.00025-0.0006, 0.00025-0.0007, 0.00025-0.0008, or 0.00025-0.001, etc.
During the preparation process, the parameters are preferably as follows: such as compression, at a pressure in the range of 5-20MPa, such as 10 MPa.
Setting parameters during reaction: in the high temperature reaction, the flow rate of the reducing atmosphere is 0.05 to 0.2L/min, preferably 0.1L/min. The reaction temperature is 1400 ℃ and 1600 ℃, the reaction temperature is preferably 1500 ℃, and the reaction time is 8-12h, preferably 10 h.
The reducing atmosphere is formed by mixing inert gas and reducing gas, wherein the reducing gas accounts for 3-6% of the total gas, preferably 3-4%, 4-5%, 5-6%, and specifically 5% by volume.
The reducing gas is preferably hydrogen.
The method of pulverization is various, and a mode of grinding and pulverization is preferable.
The application document provides a preparation method of magnesium tantalate, which comprises the steps of pressing raw materials required for synthesizing magnesium tantalate into sheets, placing the sheets in a reducing atmosphere, reacting at 1400-1600 ℃ for 8-12h, and crushing.
The magnesium tantalate is synthesized in the reducing atmosphere, and through detection, the luminescence at 460nm can be enhanced, the luminescence at 365nm can be reduced, and then the white light formed by the luminescence at 460nm and 680nm is formed, and the color coordinate is close to the standard white light.
Preferably, the reducing atmosphere is formed by mixing inert gas and reducing gas, wherein the reducing gas accounts for 3-6% of the total gas by volume, and the flow rate of the reducing atmosphere is 0.05-0.2L/min. Preferably, the reducing gas comprises hydrogen.
Further, the raw material includes an oxide or a compound of an element in the chemical formula.
Preferably, the raw material is Ta2O5And MgO, the MgO and Ta2O5The molar ratio of (A) is 4-4.08, preferably 4-4.04, or 4-4.05, or 4-4.06, or 4-4.03, or 4-4.02, etc.
Compared with the prior art, the invention has the beneficial effects that:
1. the Tb is added in the process of solid-phase synthesis of magnesium tantalate in reducing atmosphere, the white light emitted by the synthesized fluorescent powder is a color coordinate close to pure white light, the improvement effect is obvious, the process flow is simple, the controllability is strong, the selectable raw materials are rich, the replaceability is strong, the cost is low, and the yield is high.
2. The magnesium tantalate is synthesized in the reducing atmosphere, so that the emitted light is closer to the color coordinate of pure white light, and the preparation method has the advantages of simple process, strong controllability, rich raw materials, strong replaceability, low cost and high yield.
Drawings
FIG. 1 is an XRD spectrum of samples obtained in examples 2-8;
FIG. 2 is a PLE spectrum of samples obtained in examples 1-8;
FIG. 3 is a PL spectrum of samples obtained in examples 1-8;
FIG. 4 is the CIE coordinates of the samples obtained in examples 1-4.
FIG. 5 is the CIE coordinates of the samples obtained in examples 5-8.
In the drawings:
in FIGS. 2-5, 1 represents YAG prepared in example 1: ce, PDF (#79-0380) in curve 1 in FIG. 1 represents Mg4Ta2O9XRD standard card of (1);
2 in FIGS. 1-5 represents Mg prepared in example 24Ta2O9 N2；
3 represents Mg prepared in example 34Ta2O9 H2 min；
4 represents Mg prepared in example 44Ta2O9 H2 mid；
5 represents Mg prepared in example 54Ta2O9 H2 max；
6 represents Mg prepared in example 64Ta1.999O9：Tb0.01 H2；
7 represents Mg prepared in example 74Ta1.998O9：Tb0.02 H2；
8 represents Mg prepared in example 84Ta1.994O9：Tb0.06 H2。
Detailed Description
The invention is further described with reference to the following figures and specific examples.
First, sample preparation
Example 1
At room temperature, taking alumina, yttrium oxide and cerium oxide according to the element molar ratio of 2.997:5:0.003 and ethanol as a mixing medium, stirring uniformly, drying at 80 ℃, and pressing and forming at 10Mpa and 15 ℃.
And (4) reacting for 10 hours in a muffle furnace at 1200 ℃, and finishing the reaction.
After the reaction is finished, crushing and grinding the materials generated by the reaction for 20min to obtain the final white light fluorescent powder.
Example 2
First, MgO and Ta are mixed at room temperature2O5Uniformly mixing according to a molar ratio of 4.04:1, taking ethanol as a mixing medium, uniformly stirring, drying at 80 ℃, and performing compression molding under 10 Mpa;
secondly, the pressed tablets are placed in a muffle furnace and a protective atmosphere (N) with a flow rate of 0.1L/min is introduced2) Reacting for 10 hours at 1500 ℃, and finishing the reaction;
and thirdly, cooling the reaction product, and then grinding the magnesium tantalate generated by the reaction for 20min to obtain the final white-light fluorescent powder.
Example 3
First, MgO and Ta are mixed at room temperature2O5Uniformly mixing according to a molar ratio of 4:1, taking ethanol as a mixing medium, uniformly stirring, drying at 80 ℃, and performing compression molding under 5 Mpa;
secondly, the pressed tablets are placed in a muffle furnace and a weakly reducing atmosphere (Ar + 3% H) with a flow rate of 0.05L/min is introduced2) Reacting for 8 hours at 1400 ℃ and finishing the reaction;
and thirdly, cooling the reaction product, and then grinding the magnesium tantalate generated by the reaction for 20min to obtain the final white-light fluorescent powder.
Example 4
First, MgO and Ta are mixed at room temperature2O5Uniformly mixing according to a molar ratio of 4.04:1, taking ethanol as a mixing medium, uniformly stirring, drying at 80 ℃, and performing compression molding under 10 Mpa;
secondly, the pressed tablets are placed in a muffle furnace and a weakly reducing atmosphere (Ar + 5% H) with a flow rate of 0.1L/min is introduced2) Reacting for 10 hours at 1500 ℃, and finishing the reaction;
and thirdly, cooling the reaction product, and then grinding the magnesium tantalate generated by the reaction for 20min to obtain the final white-light fluorescent powder.
Example 5
First, MgO and Ta are mixed at room temperature2O5Uniformly mixing according to a molar ratio of 4.08:1, taking ethanol as a mixing medium, uniformly stirring, drying at 80 ℃, and performing compression molding under 20 Mpa;
secondly, the pressed tablets are placed in a muffle furnace and a weakly reducing atmosphere (Ar + 6% H) with a flow rate of 0.2L/min is introduced2) Reacting for 12 hours at 1600 ℃ and finishing the reaction;
and thirdly, cooling the reaction product, and then grinding the magnesium tantalate generated by the reaction for 20min to obtain the final white-light fluorescent powder.
Example 6
This embodiment is different from embodiment 4 in that: tb is added in the raw material mixture4O7，Tb4O7And Ta2O5Is 0.00025.
Example 7
This embodiment is different from embodiment 4 in that: tb is added in the raw material mixture4O7，Tb4O7And Ta2O5Is 0.0005.
Example 8
This embodiment is different from embodiment 4 in that: tb is added in the raw material mixture4O7，Tb4O7And Ta2O5Is 0.0015.
Second, performance detection
The phosphors prepared in examples 1 to 8 were examined.
As shown in FIGS. 1 to 5, the PLE spectrum of the sample prepared in example 1 has the strongest absorption peak at 465nm and has a luminescence peak between the visible light region of 500-650nm in the PL spectrum, wherein the laser peak and the emission peak are combined to form white light having color coordinates CIE (0.3567,0.4266) corresponding to a color temperature of 5046K.
As shown in FIGS. 1-4, the phosphor magnesium tantalate samples prepared in example 2 are hexagonal corundum structures; the PLE spectrum of the magnesium tantalate has the strongest absorption peak between 250-320nm, which shows that the magnesium tantalate can generate white light through the excitation of an ultraviolet-near ultraviolet chip; the PL spectrum of magnesium tantalate has predominantly 675nm emission with CIE color coordinates (0.6489,0.2914) and a corresponding color temperature of < 1000K.
As shown in FIGS. 1 to 5, the phosphor samples prepared in example 3 had a hexagonal corundum structure; but the PLE spectrum of the sample is shifted to the long wavelength direction and still is between 250-320nm, and white light can be generated by the excitation of an ultraviolet-near ultraviolet chip; the PL spectrum of the magnesium tantalate has a luminescence peak between 380-800nm visible light, and has two luminescence peaks at 460nm and 680 nm. The color coordinates CIE of the white light are calculated to be (0.3512,0.3099), the corresponding color temperature is 4980K, and compared with the sample in the embodiment 2, the color coordinates of the sample white light in the embodiment are improved remarkably.
As shown in FIGS. 1 to 5, the phosphor samples prepared in example 4 have a hexagonal corundum structure; but the PLE excitation peak of the sample is between 250-320nm, and white light can be generated by ultraviolet-near ultraviolet chip excitation; the PL spectrum of the magnesium tantalate has a luminescence peak between 380-800nm visible light, and has two luminescence peaks at 460nm and 680 nm. The color coordinates CIE of the white light are calculated to be (0.3313,0.3125), the corresponding color temperature is 5891K, and the color coordinates of the sample white light in this embodiment are further improved compared with the sample in embodiment 3.
As shown in FIGS. 1 to 5, the phosphor samples prepared in example 5 have a hexagonal corundum structure; but the PLE excitation peak of the sample is between 250-320nm, and white light can be generated by ultraviolet-near ultraviolet chip excitation; the PL spectrum of the magnesium tantalate emits light at 460nm and 680 nm. The color coordinates of the white light were calculated to be CIE (0.2642,0.275) and correspond to a color temperature of >10000K, which is far from standard white light compared to the sample of example 4.
As shown in fig. 1 to 5, the present embodiment 6 differs from the embodiment 4 in that: the PL spectrum shows characteristic peaks for Tb ions. The color coordinates CIE of the white light are calculated to be (0.3308,0.3205), and the corresponding color temperature is 5575K. It can be seen that the samples prepared in this example further approach pure white light (0.33 ).
As shown in fig. 1 to 5, the present embodiment 7 differs from embodiment 6 in that: the characteristic peak of Tb ion in PL spectrum is further enhanced. Through calculation of the color coordinates CIE of the white light to be (0.3307,0.3298), and the corresponding color temperature to be 5575K, it can be seen that the color coordinates (0.33 ) of the sample prepared in this embodiment are already close to those of pure white light.
As shown in fig. 1 to 5, the present embodiment 8 differs from embodiment 7 in that: the characteristic peak of Tb ion in the PL spectrum reaches a maximum. The color coordinates of the white light were calculated to have CIE of (0.3303,0.3532) and a corresponding color temperature of 5589K, which is far from the standard white light compared to the sample of example 7.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-mentioned embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (10)
1. A preparation method of white light fluorescent powder is characterized by comprising the following steps: the method comprises the following steps:
mixing and tabletting raw materials required for synthesis;
placing the pressed body in a reducing atmosphere, and reacting for 8-12h at the temperature of 1400 ℃ and 1600 ℃;
crushing the cooled pressed sheet to obtain the fluorescent powder, wherein the chemical structural formula of the fluorescent powder is Mg4Ta2-xO9：Tbx，0.001≤X≤0.006。
2. The method of claim 1, wherein: the raw material comprises an oxide or a compound of an element in the chemical formula.
3. The method of claim 2, wherein: the raw material is Ta2O5、Tb4O7And MgO, the MgO and Ta2O5In a molar ratio of 4 to 4.08, Tb4O7And Ta2O5The molar ratio of (A) is 0.00025-0.0015.
4. The method of claim 1, wherein: the reducing atmosphere is formed by mixing inert gas and reducing gas, wherein the reducing gas accounts for 3-6% of the total gas by volume, and the flow of the reducing atmosphere is 0.05-0.2L/min.
5. The method of claim 4, wherein: the reducing gas comprises hydrogen.
6. A method for preparing magnesium tantalate is characterized in that: pressing raw materials required for synthesizing the magnesium tantalate into tablets, placing the tablets in a reducing atmosphere, reacting for 8-12h at the temperature of 1400 ℃ and 1600 ℃, and crushing.
7. The method of claim 6, wherein: the reducing atmosphere is formed by mixing inert gas and reducing gas, wherein the reducing gas accounts for 3-6% of the total gas by volume, and the flow of the reducing atmosphere is 0.05-0.2L/min.
8. The method of claim 7, wherein: the reducing gas comprises hydrogen.
9. The method of claim 6, wherein: the raw material comprises an oxide or a compound of an element in the chemical formula.
10. The method of claim 9, wherein: the raw material is Ta2O5And MgO, the MgO and Ta2O5Is 4 to 4.08.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113563881A (en) * | 2021-08-10 | 2021-10-29 | 上海应用技术大学 | Rare earth doped magnesium tantalate scintillation luminescent material and preparation method thereof |
| CN114106828A (en) * | 2021-12-20 | 2022-03-01 | 内蒙古大学 | Cr (chromium)3+Doped near-infrared fluorescent powder with broadband emission and preparation method thereof |
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| CN103191716A (en) * | 2013-04-17 | 2013-07-10 | 桂林理工大学 | Corundum structured composite oxide photocatalyst Mg4Nb2-xTaxO9 and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113563881A (en) * | 2021-08-10 | 2021-10-29 | 上海应用技术大学 | Rare earth doped magnesium tantalate scintillation luminescent material and preparation method thereof |
| CN113563881B (en) * | 2021-08-10 | 2023-08-18 | 上海应用技术大学 | Rare earth doped magnesium tantalate scintillation luminescent material and preparation method thereof |
| CN114106828A (en) * | 2021-12-20 | 2022-03-01 | 内蒙古大学 | Cr (chromium)3+Doped near-infrared fluorescent powder with broadband emission and preparation method thereof |
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