CN111410959A - Rare earth phosphate-based orange red fluorescent powder and preparation method thereof - Google Patents
Rare earth phosphate-based orange red fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
A rare earth phosphate-based orange red fluorescent powder with a chemical formula of RbSrGd and a preparation method thereof1‑xEux(PO4)2，Wherein x = 0.02, 0.04, 0.06, 0.08, 0.1, 0.12, 0.14, 0.15. System for making The preparation method comprises the following steps:weighing rubidium chloride, strontium carbonate, gadolinium oxide, europium oxide and diammonium phosphate, wherein the mass ratio of the rubidium chloride to the strontium carbonate to the gadolinium oxide to the europium oxide to the diammonium phosphate is 19: 19: 9.5 (1-x): 9.5 x: 38, wherein x =0.02, 0.04, 0.06, 0.08, 0.1, 0.12, 0.14 or 0.15, grinding and mixing uniformly, heating to 970 ℃ -990 ℃ in a box type resistance furnace under the air atmosphere, preserving heat for 6-10h, cooling to room temperature along with the furnace, taking out and grinding to obtain the product. The invention has simple preparation method, low preparation temperature, high emission intensity and stable performance, and Eu is used3+The fluorescent powder is used as a main activator, has wide excitable light wavelength range, can be effectively excited by near ultraviolet light or blue light emitted by a semiconductor L ED chip, presents sharp spectral line emission and belongs to an orange red light range, and the fluorescent powder is used at 39The light with the wavelength of 3nm can emit bright orange-red light under the excitation.
Description
Technical Field
The invention belongs to the technical field of fluorescent materials of light emitting diodes, and particularly relates to rare earth phosphate-based orange red fluorescent powder and a preparation method of the fluorescent powder.
Background
In recent years, a light emitting diode (L ED) is considered as a new generation green illumination light source capable of replacing a traditional incandescent lamp and a mercury-containing fluorescent lamp due to the advantages of low power consumption, energy conservation, environmental protection, severe environment resistance, long service life, high luminous efficiency, high response speed, small volume, long visual distance and the like, a L ED light source which is mainstream in the current market is a fluorescence conversion type white light L ED, and the mode of utilizing a fluorescent material and a L ED chip to form a device to realize white light mainly comprises a blue light L ED + yellow fluorescent material, a blue light L ED + green and red fluorescent material and (near) ultraviolet L ED + red green blue three-primary-color fluorescent powder, wherein the fluorescent powder plays a vital role in three schemes, so that the development of the novel high-performance fluorescent powder is a necessary condition for the development of the fluorescence conversion type white light L ED4And EuPO4Research on fluorescence properties, researchers have done a lot of research works on rare earth phosphate luminescent materials so far, and luminescent materials using rare earth phosphate as a matrix have potential application value in the field of green lighting.
But Eu3+Doped RbSrGd (PO)4)2The fluorescent powder has not been reported before, and can emit bright orange-red light under the excitation of 393nm wavelength light.
Disclosure of Invention
The invention aims to provide rare earth phosphate-based orange red fluorescent powder and a preparation method thereof, and the fluorescent powder has stable chemical properties, high luminous intensity and warm tone, and can be effectively excited by near ultraviolet light (393 nm) to emit visible light.
The object of the invention is achieved in the following way:
a rare earth phosphate-based orange red fluorescent powder is characterized in that: the chemical formula is RbSrGd1-xEux(PO4)2Wherein x =0.02, 0.04、0.06、0.08、0.1、0.12、0.14、0.15。
The rare earth phosphate-based orange red fluorescent powder is prepared from rare earth phosphate RbSrGd (PO)4)2For the matrix, Eu was doped at 2 at.%, 4at.%, 6 at.%, 8 at.%, 10 at.%, 12 at.%, 14at.%, and 15 at.%, respectively3+Occupies Gd3+Obtaining the rare earth phosphate-based orange red fluorescent powder at the lattice site.
The rare earth phosphate-based orange red fluorescent powder, the Eu3 +Occupying symmetric sites in the host lattice.
The rare earth phosphate-based orange red fluorescent powder is prepared from the rare earth phosphate RbSrGd (PO)4)2The matrix belongs to the P6222 (No. 180) space group, hexagonal system.
A preparation method of rare earth phosphate-based orange red fluorescent powder comprises the following steps of weighing rubidium chloride, strontium carbonate, gadolinium oxide, europium oxide and diammonium phosphate, wherein the mass ratio of the rubidium chloride to the strontium carbonate to the gadolinium oxide to the europium oxide to the diammonium phosphate is 19: 19: 9.5 (1-x): 9.5 x: 38, wherein x =0.02, 0.04, 0.06, 0.08, 0.1, 0.12, 0.14 or 0.15, grinding and mixing uniformly, heating to 970 ℃ -990 ℃ in a box type resistance furnace under the air atmosphere, preserving heat for 6-10h, cooling to room temperature along with the furnace, taking out and grinding to obtain the product.
A method for preparing rare earth phosphate-based orange red fluorescent powder comprises weighing rubidium chloride (RbCl) and strontium carbonate (SrCO)3) Gadolinium oxide (Gd)2O3) Europium oxide (Eu)2O3) Diammonium hydrogen phosphate ((NH)4)2HPO4) Wherein rubidium chloride (RbCl), strontium carbonate (SrCO)3) Gadolinium oxide (Gd)2O3) Europium oxide (Eu)2O3) Diammonium hydrogen phosphate ((NH)4)2HPO4) The mass ratio of (a) to (b) is 19: 19: 9 (1-x): 9 x: 38, wherein x =0.02, 0.04, 0.06, 0.08, 0.1, 0.12, 0.14 or 0.15, grinding and mixing uniformly, heating to 970 ℃ -990 ℃ in a box type resistance furnace under the air atmosphere, preserving heat for 6-10h, cooling to room temperature along with the furnace, taking out and grinding to obtain the product.
The preparation method of the rare earth phosphate orange-red fluorescent powder comprises the steps of heating to 980 ℃ in a box type resistance furnace in the air atmosphere, preserving heat for 8 hours, cooling to room temperature along with the furnace, taking out and grinding to obtain the product.
Compared with the prior art, the invention has the following beneficial effects: simple preparation method, low preparation temperature, high emission intensity and stable performance, and uses Eu as raw material3+The active component is a main activator, has wide wavelength range of excitable light, can be effectively excited by near ultraviolet light or blue light emitted by a semiconductor L ED chip, presents sharp spectral line emission and belongs to the orange red light range3+Doped RbSrGd (PO)4)2The fluorescent powder has not been reported before, can emit bright orange-red light under the excitation of 393nm wavelength light, and can be applied to the field of L ED green illumination.
Drawings
FIG. 1 is the XRD pattern of example 1;
FIG. 2 is a Scanning Electron Microscope (SEM) image of example 1;
FIG. 3 the emission spectrum of the product obtained in example 1 at 393nm excitation;
FIG. 4 shows RbSrGd (PO)4)2:15%Eu3+A color coordinate map of the phosphor;
FIG. 5 shows that the product obtained in example 1 was tested for RbSrGd (PO) at 586 nm wavelength monitoring4)2:2%Eu3+The excitation spectrum of (1);
FIG. 6 is a test chart of the emission spectra of the product obtained in example 1 under the excitation of ultraviolet light with different wavelengths.
Detailed Description
Example 1:
RbSrGd0.98Eu0.02(PO4)2phosphor synthesis:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2302g of rubidium chloride (RbCl) and 0.2818g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.3391g gadolinium oxide (Gd)2O3) 0.0068g of europium oxide (Eu)2O3) 0.5028g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing in agate mortar, adding appropriate amount of anhydrous ethanol dropwise, and grindingUniformly mixing the raw materials, heating the mixture to 980 ℃ in a box type resistance furnace in the air atmosphere, preserving the heat for 8 hours, cooling the mixture to room temperature along with the furnace, taking out the mixture, and grinding the mixture to obtain the product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 2:
RbSrGd0.96Eu0.04(PO4)2phosphor synthesis:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2314g of rubidium chloride (RbCl) and 0.2828g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.3307g gadolinium oxide (Gd)2O3) 0.0136g of europium oxide (Eu)2O3) 0.5058g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing the mixture into an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding to uniformly mix the raw materials, heating the mixture to 980 ℃ in a box type resistance furnace under the air atmosphere, preserving the heat for 8 hours, cooling the mixture to room temperature along with the furnace, taking out and grinding to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 3:
RbSrGd0.94Eu0.06(PO4)2phosphor synthesis:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2307g of rubidium chloride (RbCl) and 0.2819g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.3236g gadolinium oxide (Gd)2O3) 0.0210g of europium oxide (Eu)2O3) 0.5032g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing the mixture into an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding to uniformly mix the raw materials, heating the mixture to 980 ℃ in a box type resistance furnace under the air atmosphere, preserving the heat for 8 hours, cooling the mixture to room temperature along with the furnace, taking out and grinding to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 4:
RbSrGd0.92Eu0.08(PO4)2phosphor synthesis:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2312g of rubidium chloride (RbCl) and 0.2828g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.3178g gadolinium oxide (Gd)2O3) 0.0275g of europium oxide (Eu)2O3) 0.5034g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing the mixture into an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding to uniformly mix the raw materials, heating the mixture to 980 ℃ in a box type resistance furnace under the air atmosphere, preserving the heat for 8 hours, cooling the mixture to room temperature along with the furnace, taking out and grinding to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 5:
RbSrGd0.9Eu0.1(PO4)2phosphor:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2315g of rubidium chloride (RbCl) and 0.2828g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.31g of gadolinium oxide (Gd)2O3) 0.0334g of europium oxide (Eu)2O3) 0.5026g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing the mixture into an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding to uniformly mix the raw materials, heating the mixture to 980 ℃ in a box type resistance furnace under the air atmosphere, preserving the heat for 8 hours, cooling the mixture to room temperature along with the furnace, taking out and grinding to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 6:
RbSrGd0.88Eu0.12(PO4)2phosphor:
0.2311g of rubidium chloride (RbCl) and 0.2823g of strontium carbonate (SrCO) are sequentially weighed by adopting a high-temperature solid-phase reaction method and taking 1g of synthesized product as a reference3) 0.3031g gadolinium oxide (Gd)2O3) 0.0401g of europium oxide (Eu)2O3) 0.5037g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing the mixture into an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding to uniformly mix the raw materials, heating the mixture to 980 ℃ in a box type resistance furnace under the air atmosphere, preserving the heat for 8 hours, cooling the mixture to room temperature along with the furnace, taking out and grinding to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 7:
RbSrGd0.86Eu0.14(PO4)2phosphor synthesis:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2309g of rubidium chloride (RbCl) and 0.2812g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.2962g gadolinium oxide (Gd)2O3) 0.0468g of europium oxide (Eu)2O3) 0.5030g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing the mixture into an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding to uniformly mix the raw materials, heating the mixture to 980 ℃ in a box type resistance furnace under the air atmosphere, preserving the heat for 8 hours, cooling the mixture to room temperature along with the furnace, taking out and grinding to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 8:
RbSrGd0.85Eu0.15(PO4)2phosphor synthesis:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2298g of rubidium chloride (RbCl) and 0.2810g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.2927g gadolinium oxide (Gd)2O3) 0.0503g of europium oxide (Eu)2O3) 0.5028g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing the mixture into an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding to uniformly mix the raw materials, heating the mixture to 980 ℃ in a box type resistance furnace under the air atmosphere, preserving the heat for 8 hours, cooling the mixture to room temperature along with the furnace, taking out and grinding to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 9:
RbSrGd0.98Eu0.02(PO4)2phosphor synthesis:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2297g of rubidium chloride (RbCl) and 0.2805g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.3197g gadolinium oxide (Gd)2O3) 0.0063g of europium oxide (Eu)2O3) 0.5018g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing in agate mortar, adding appropriate amount of anhydrous ethanol dropwise, grinding thoroughly to mix the raw materials, heating in box-type resistance furnace under air atmosphere to970 ℃, keeping the temperature for 6h, cooling to room temperature along with the furnace, taking out and grinding to obtain the product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 10:
RbSrGd0.96Eu0.04(PO4)2phosphor synthesis:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2297g of rubidium chloride (RbCl) and 0.2805g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.3136g gadolinium oxide (Gd)2O3) 0.0127g of europium oxide (Eu)2O3) 0.5018g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing the mixture into an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding the mixture to uniformly mix the raw materials, heating the mixture to 975 ℃ in a box-type resistance furnace under the air atmosphere, preserving the heat for 7 hours, cooling the mixture to room temperature along with the furnace, taking out the mixture, and grinding the mixture to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 11:
RbSrGd0.94Eu0.06(PO4)2phosphor synthesis:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2297g of rubidium chloride (RbCl) and 0.2805g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.3367g gadolinium oxide (Gd)2O3) 0.0190g of europium oxide (Eu)2O3) 0.5032g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing in an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding to uniformly mix the raw materials, heating to 985 ℃ in a box type resistance furnace under the air atmosphere, preserving heat for 8.5h, cooling to room temperature along with the furnace, taking out and grinding to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 12:
RbSrGd0.92Eu0.08(PO4)2phosphor synthesis:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2297g of rubidium chloride (RbCl) and 0.2805g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.3030g gadolinium oxide (Gd)2O3) 0.0253g of oxygenEuropium oxide (Eu)2O3) 0.5018g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing the mixture into an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding to uniformly mix the raw materials, heating the mixture to 987 ℃ in a box type resistance furnace under the air atmosphere, preserving the heat for 9 hours, cooling the mixture to room temperature along with the furnace, taking out and grinding to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 13:
RbSrGd0.9Eu0.1(PO4)2phosphor:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2297g of rubidium chloride (RbCl) and 0.2805g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.2936g gadolinium oxide (Gd)2O3) 0.0317g of europium oxide (Eu)2O3) 0.5018g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing in an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding to uniformly mix the raw materials, heating to 989 ℃ in a box type resistance furnace under the air atmosphere, preserving heat for 9.5 hours, cooling to room temperature along with the furnace, taking out and grinding to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 14:
RbSrGd0.88Eu0.12(PO4)2phosphor:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2297g of rubidium chloride (RbCl) and 0.2805g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.2871g gadolinium oxide (Gd)2O3) 0.0380g of europium oxide (Eu)2O3) 0.5018g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing the mixture into an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding to uniformly mix the raw materials, heating the mixture to 990 ℃ in a box-type resistance furnace under the air atmosphere, preserving the heat for 10 hours, cooling the mixture to room temperature along with the furnace, taking out the mixture, and grinding to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 15:
RbSrGd0.86Eu0.14(PO4)2phosphor synthesis:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2297g of rubidium chloride (RbCl) and 0.2805g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.2806g gadolinium oxide (Gd)2O3) 0.0443g of europium oxide (Eu)2O3) 0.5018g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing the mixture into an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding to uniformly mix the raw materials, heating the mixture to 980 ℃ in a box type resistance furnace under the air atmosphere, preserving the heat for 8 hours, cooling the mixture to room temperature along with the furnace, taking out and grinding to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
Example 16:
RbSrGd0.85Eu0.15(PO4)2phosphor synthesis:
adopting a high-temperature solid-phase reaction method, and sequentially weighing 0.2297g of rubidium chloride (RbCl) and 0.2805g of strontium carbonate (SrCO) based on 1g of synthesized product3) 0.2773g gadolinium oxide (Gd)2O3) 0.0475g of europium oxide (Eu)2O3) 0.5018g of diammonium hydrogen phosphate ((NH)4)2HPO4) Placing the mixture into an agate mortar, dropwise adding a proper amount of absolute ethyl alcohol, fully grinding the mixture to enable the raw materials to be uniformly mixed, heating the mixture to 975 ℃ in a box-type resistance furnace under the air atmosphere, preserving the heat for 7.5 hours, cooling the mixture to room temperature along with the furnace, taking out the mixture, and grinding the mixture to obtain a product. The temperature rise speed of the box-type resistance furnace is 10 ℃/min.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the overall concept of the invention, and these should be considered as the protection scope of the present invention, which will not affect the effect of the implementation of the present invention and the practicability of the patent.
Claims (7)
1. A rare earth phosphate-based orange red fluorescent powder is characterized in that: the chemical formula is RbSrGd1-xEux(PO4)2Wherein x =0.02, 0.04, 0.06, 0.08, 0.1, 0.12, 0.14, 0.15.
2. The rare earth phosphate-based orange-red phosphor of claim 1, wherein: with rare earth phosphate RbSrGd (PO)4)2For the matrix, Eu was doped at 2 at.%, 4at.%, 6 at.%, 8 at.%, 10 at.%, 12 at.%, 14at.%, and 15 at.%, respectively3+Occupies Gd3+Obtaining the rare earth phosphate-based orange red fluorescent powder at the lattice site.
3. The rare earth phosphate-based orange-red phosphor of claim 1, wherein: the Eu being3 +Occupying symmetric sites in the host lattice.
4. The rare earth phosphate-based orange-red phosphor of claim 1, wherein: the rare earth phosphate RbSrGd (PO)4)2The matrix belongs to the P6222 (No. 180) space group, hexagonal system.
5. A preparation method of rare earth phosphate-based orange red fluorescent powder is characterized by comprising the following steps: weighing rubidium chloride, strontium carbonate, gadolinium oxide, europium oxide and diammonium phosphate, wherein the mass ratio of the rubidium chloride to the strontium carbonate to the gadolinium oxide to the europium oxide to the diammonium phosphate is 19: 19: 9.5 (1-x): 9.5 x: 38, wherein x =0.02, 0.04, 0.06, 0.08, 0.1, 0.12, 0.14 or 0.15, grinding and mixing uniformly, heating to 970 ℃ -990 ℃ in a box type resistance furnace under the air atmosphere, preserving heat for 6-10h, cooling to room temperature along with the furnace, taking out and grinding to obtain the product.
6. A preparation method of rare earth phosphate-based orange red fluorescent powder is characterized by comprising the following steps: weighing rubidium chloride, strontium carbonate, gadolinium oxide, europium oxide and diammonium phosphate, wherein the mass ratio of the rubidium chloride to the strontium carbonate to the gadolinium oxide to the europium oxide to the diammonium phosphate is 19: 19: 9 (1-x): 9 x: 38, wherein x =0.02, 0.04, 0.06, 0.08, 0.1, 0.12, 0.14 or 0.15, grinding and mixing uniformly, heating to 970 ℃ -990 ℃ in a box type resistance furnace under the air atmosphere, preserving heat for 6-10h, cooling to room temperature along with the furnace, taking out and grinding to obtain the product.
7. The method for preparing rare earth phosphate orange-red fluorescent powder according to claim 5 or 6, characterized in that: heating to 980 ℃ in a box type resistance furnace under the air atmosphere, preserving heat for 8h, cooling to room temperature along with the furnace, taking out and grinding to obtain the product.
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