CN108456523B - Fluorescent powder for LED lamp for plant growth and preparation method thereof - Google Patents
Fluorescent powder for LED lamp for plant growth and preparation method thereof Download PDFInfo
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- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
- C09K11/71—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus also containing alkaline earth metals
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7715—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing cerium
- C09K11/7723—Phosphates
- C09K11/7724—Phosphates with alkaline earth metals
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- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
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Abstract
The invention relates to the technical field of rare earth luminescent materials. The fluorescent powder for the LED lamp for plant growth has the following chemical expression: (Ba)0.5‑x‑yMgy)M2(PO4)3：xMn2+Wherein M is any one of Zr, Ce and Hf, x is 0.001-0.1, and y is 0.05-0.2. The fluorescent powder can realize multicolor luminescence based on a single substrate, and the emitted light is respectively positioned in blue light, red light and near infrared light regions, thereby being beneficial to plant growth.
Description
Technical Field
The invention relates to the technical field of rare earth luminescent materials, in particular to fluorescent powder for a plant growth LED lamp and a preparation method thereof.
Background
Illumination has been of great interest to academic researchers as a source of energy for plant photosynthesis. In recent years, researchers have studied the influence of different light on plant growth, so as to analyze the spectral composition of absorption spectra of different light receptors, find a luminescent material with an emission spectrum matched with light required by plant growth, and achieve the purpose of improving photosynthesis efficiency. An make internal disorder or usurp research shows that blue light (400-500 nm) can promote stem leaf growth, red light (600-800 nm) can regulate flowering period, and near infrared light (850-1100 nm) has regulation and control effects on root growth and nutrient absorption. If a light source with blue, red and near infrared light emission is artificially provided to an indoor planting system with controllable environment, the growth state of organisms planted therein will be optimized. In short, the spectrum composition of the artificial light source can be regulated and controlled to effectively regulate the morphogenesis and growth and development processes of plants, thereby achieving the purpose of improving the yield and quality of crops. In the light conversion type plant growth LED lamp, a near ultraviolet or blue light chip is required to excite a mixture of single-color fluorescent powder or single-matrix multicolor fluorescent powder, and the fluorescent powder needs to have three conditions: firstly, the chip has stronger absorption in a near ultraviolet or blue light region, namely the excitation spectrum of the chip is matched with the chip; the blue light, the red light or the near infrared light can be emitted under the excitation of the near ultraviolet light or the blue light; thirdly, physical and chemical stability is high, low cost and easy synthesis.
Disclosure of Invention
The invention aims to provide the fluorescent powder for the plant growth LED lamp, which has high luminous brightness and luminous efficiency, stable physical and chemical properties, and favorable plant growth because the emitted light is respectively positioned in blue light, red light and near infrared light regions, and the preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the fluorescent powder for the LED lamp for plant growth has the following chemical expression: (Ba)0.5-x-yMgy)M2(PO4)3：xMn2+Wherein M is any one of Zr, Ce and Hf, x is 0.001-0.1, and y is 0.05-0.2.
A preparation method of fluorescent powder for a plant growth LED lamp comprises the following steps:
(1) with barium carbonate, magnesium carbonate, M-containing oxide, [ PO ]4]3-Compound and manganese carbonate according to the chemical formula (Ba)0.5-x-yMgy)M2(PO4)3：xMn2+Wherein M is any one of Zr, Ce and Hf, x is 0.001-0.1, and y is 0.05-0.2 to obtain a mixture; (2) mixing the mixtureAnd (3) putting the mixture into a crucible, sintering the mixture for 2 to 4 hours in a high-temperature furnace at the temperature of 1300 to 1400 ℃ in a protective atmosphere, and cooling the mixture to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
Further, the compound containing M is any one of zirconium oxide, cerium oxide and hafnium oxide.
Further, the [ PO ] containing4]3-The compound is one of diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
Further, the protective atmosphere is nitrogen or argon atmosphere.
Compared with the prior art, the invention has the beneficial effects that: (1) the phosphor powder of the invention takes phosphate as a matrix material, and has the advantages of good chemical stability, good thermal stability, low price of raw materials, rich reserves, low sintering temperature and the like. Compared with sulfide fluorescent powder, the invention has good thermal stability. Compared with silicate fluorescent powder, the invention has uniform particle size and lower sintering temperature. Compared with silicon-based nitrogen (oxygen) compound fluorescent powder, the invention has the advantages of simple synthesis process, low sintering temperature, low raw material price and abundant reserves. Compared with aluminate fluorescent powder, the invention has the advantages of low preparation temperature, small particle size, high luminous brightness and luminous efficiency and stable physical and chemical properties. (2) The fluorescent powder can realize multicolor luminescence based on a single substrate, and the emitted light is respectively positioned in blue light, red light and near infrared light regions, thereby being beneficial to plant growth.
Drawings
FIG. 1 is an excitation spectrum of the phosphor prepared in example 1 according to the present invention.
FIG. 2 is an emission spectrum of the phosphor prepared in example 1 according to the present invention.
FIG. 3 shows the XRD pattern and standard pattern of the phosphor prepared in example 1.
Detailed Description
The patent is described in detail below with reference to the drawings and examples.
Example 1
The fluorescent powder for the LED lamp for plant growth has the following chemical expression: (Ba)0.35Mg0.05)Zr2(PO4)3：0.1Mn2+。
According to (Ba)0.35Mg0.05)Zr2(PO4)3：0.1Mn2+Weighing BaCO3、MgCO3、ZrO2、(NH4)2HPO4And MnCO3And the molar ratio between them is 0.35: 0.05: 2: 3: 0.1, fully grinding and uniformly mixing, placing into a corundum crucible, placing into a high-temperature furnace, roasting at 1400 ℃ for 2 hours in a nitrogen atmosphere, and then cooling to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
Fig. 1 is an excitation spectrum of the phosphor prepared in this example, with a monitoring wavelength of 610 nm, and it can be seen from fig. 1 that the excitation spectrum of the phosphor of this example is a broad spectrum covering the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, which illustrates that the phosphor of this example can be effectively excited by the ultraviolet and violet chips. FIG. 1 is an emission spectrum of the phosphor prepared in this example, wherein the excitation wavelength is 350 nm, and under 360nm light excitation, as can be seen from FIG. 2, the phosphor of this example emits blue light, red light and near infrared light, and the emission peaks are respectively located near 450nm, 610 nm and 750nm, which indicates that the phosphor of this example is suitable for being used as a single-matrix multicolor phosphor. FIG. 3 is the XRD pattern and standard pattern (ICSD: 250171) of the phosphor prepared in the example, and it can be seen from FIG. 3 that the XRD pattern of the phosphor of the example shows the d value and relative intensity variation trend of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
Example 2
According to (Ba)0.2Mg0.2)Zr2(PO4)3：0.1Mn2+Weighing BaCO3、MgCO3、ZrO2、NH4H2PO4And MnCO3And the molar ratio between them is 0.2: 0.2: 2: 3: 0.1, fully grinding and uniformly mixing, placing into a corundum crucible, placing into a high-temperature furnace, roasting at 1300 ℃ for 4 hours under argon,and then cooling to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
The excitation spectrum of the phosphor of this embodiment is a broad spectrum, which covers the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, indicating that the phosphor of this embodiment can be effectively excited by the ultraviolet and violet chips. Under the excitation of 360nm light, the phosphor of the embodiment emits blue light, red light and near infrared light, and the emission peaks are respectively located near 450nm, 610 nm and 750nm, which indicates that the phosphor of the embodiment is suitable for being used as single-matrix multicolor phosphor. The XRD pattern of the phosphor powder in this example shows the d value and the trend of the relative intensity change of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
Example 3
According to (Ba)0.449Mg0.05)Zr2(PO4)3：0.001Mn2+Weighing BaCO3、MgCO3、ZrO2、(NH4)2HPO4And MnCO3And the molar ratio between them is 0.449: 0.05: 2: 3: 0.001, fully grinding and uniformly mixing, placing into a corundum crucible, placing into a high-temperature furnace, roasting at 1400 ℃ for 2 hours in a nitrogen atmosphere, and then cooling to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
The excitation spectrum of the phosphor of this embodiment is a broad spectrum, which covers the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, indicating that the phosphor of this embodiment can be effectively excited by the ultraviolet and violet chips. Under the excitation of 360nm light, the phosphor of the embodiment emits blue light, red light and near infrared light, and the emission peaks are respectively located near 450nm, 610 nm and 750nm, which indicates that the phosphor of the embodiment is suitable for being used as single-matrix multicolor phosphor. The XRD pattern of the phosphor powder in this example shows the d value and the trend of the relative intensity change of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
Example 4
According to (Ba)0.299Mg0.2)Zr2(PO4)3：0.001Mn2+Weighing BaCO3、MgCO3、ZrO2、NH4H2PO4And MnCO3And the molar ratio between them is 0.299: 0.2: 2: 3: 0.001, fully grinding and uniformly mixing, placing into a corundum crucible, placing into a high-temperature furnace, roasting at 1300 ℃ for 4 hours under the argon atmosphere, and then cooling to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
The excitation spectrum of the phosphor of this embodiment is a broad spectrum, which covers the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, indicating that the phosphor of this embodiment can be effectively excited by the ultraviolet and violet chips. Under the excitation of 360nm light, the phosphor of the embodiment emits blue light, red light and near infrared light, and the emission peaks are respectively located near 450nm, 610 nm and 750nm, which indicates that the phosphor of the embodiment is suitable for being used as single-matrix multicolor phosphor. The XRD pattern of the phosphor powder in this example shows the d value and the trend of the relative intensity change of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
Example 5
According to (Ba)0.299Mg0.1)Zr2(PO4)3：0.01Mn2+Weighing BaCO3、MgCO3、ZrO2、NH4H2PO4And MnCO3And the molar ratio between them is 0.39: 0.1: 2: 3: 0.01, fully grinding and uniformly mixing, placing into a corundum crucible, placing into a high-temperature furnace, roasting at 1350 ℃ for 3 hours under the argon atmosphere, and then cooling to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
The excitation spectrum of the phosphor of this embodiment is a broad spectrum, which covers the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, indicating that the phosphor of this embodiment can be effectively excited by the ultraviolet and violet chips. The phosphor of this example emits blue, red and near infrared light under 360nm excitationThe emission peak values are respectively located near 450nm, 610 nm and 750nm, which shows that the fluorescent powder of the embodiment is suitable for being used as single-matrix multicolor fluorescent powder. The XRD pattern of the phosphor powder in this example shows the d value and the trend of the relative intensity change of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
Example 6
According to (Ba)0.35Mg0.05)Ce2(PO4)3：0.1Mn2+Weighing BaCO3、MgCO3、CeO2、(NH4)2HPO4And MnCO3And the molar ratio between them is 0.35: 0.05: 2: 3: 0.1, fully grinding and uniformly mixing, placing into a corundum crucible, placing into a high-temperature furnace, roasting at 1400 ℃ for 2 hours in a nitrogen atmosphere, and then cooling to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
The excitation spectrum of the phosphor of this embodiment is a broad spectrum, which covers the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, indicating that the phosphor of this embodiment can be effectively excited by the ultraviolet and violet chips. Under the excitation of 360nm light, the phosphor of the embodiment emits blue light, red light and near infrared light, and the emission peaks are respectively located near 450nm, 610 nm and 750nm, which indicates that the phosphor of the embodiment is suitable for being used as single-matrix multicolor phosphor. The XRD pattern of the phosphor powder in this example shows the d value and the trend of the relative intensity change of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
Example 7
According to (Ba)0.2Mg0.2)Ce2(PO4)3：0.1Mn2+Weighing BaCO3、MgCO3、CeO2、NH4H2PO4And MnCO3And the molar ratio between them is 0.2: 0.2: 2: 3: 0.1, fully grinding and uniformly mixing, placing into a corundum crucible, and then placing into a high-temperature furnace under the argon atmosphere at 1Roasting for 4 hours at 300 ℃, and then cooling to room temperature to obtain the fluorescent powder for the LED lamp for plant growth.
The excitation spectrum of the phosphor of this embodiment is a broad spectrum, which covers the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, indicating that the phosphor of this embodiment can be effectively excited by the ultraviolet and violet chips. Under the excitation of 360nm light, the phosphor of the embodiment emits blue light, red light and near infrared light, and the emission peaks are respectively located near 450nm, 610 nm and 750nm, which indicates that the phosphor of the embodiment is suitable for being used as single-matrix multicolor phosphor. The XRD pattern of the phosphor powder in this example shows the d value and the trend of the relative intensity change of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
Example 8
According to (Ba)0.449Mg0.05)Ce2(PO4)3：0.001Mn2+Weighing BaCO3、MgCO3、CeO2、(NH4)2HPO4And MnCO3And the molar ratio between them is 0.449: 0.05: 2: 3: 0.001, fully grinding and uniformly mixing, placing into a corundum crucible, placing into a high-temperature furnace, roasting at 1400 ℃ for 2 hours in a nitrogen atmosphere, and then cooling to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
The excitation spectrum of the phosphor of this embodiment is a broad spectrum, which covers the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, indicating that the phosphor of this embodiment can be effectively excited by the ultraviolet and violet chips. Under the excitation of 360nm light, the phosphor of the embodiment emits blue light, red light and near infrared light, and the emission peaks are respectively located near 450nm, 610 nm and 750nm, which indicates that the phosphor of the embodiment is suitable for being used as single-matrix multicolor phosphor. The XRD pattern of the phosphor powder in this example shows the d value and the trend of the relative intensity change of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
Example 9
According to (Ba)0.299Mg0.2)Ce2(PO4)3：0.001Mn2+Weighing BaCO3、MgCO3、CeO2、NH4H2PO4And MnCO3And the molar ratio between them is 0.299: 0.2: 2: 3: 0.001, fully grinding and uniformly mixing, placing into a corundum crucible, placing into a high-temperature furnace, roasting at 1300 ℃ for 4 hours under the argon atmosphere, and then cooling to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
The excitation spectrum of the phosphor of this embodiment is a broad spectrum, which covers the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, indicating that the phosphor of this embodiment can be effectively excited by the ultraviolet and violet chips. Under the excitation of 360nm light, the phosphor of the embodiment emits blue light, red light and near infrared light, and the emission peaks are respectively located near 450nm, 610 nm and 750nm, which indicates that the phosphor of the embodiment is suitable for being used as single-matrix multicolor phosphor. The XRD pattern of the phosphor powder in this example shows the d value and the trend of the relative intensity change of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
Example 10
According to (Ba)0.35Mg0.05)Hf2(PO4)3：0.1Mn2+Weighing BaCO3、MgCO3、HfO2、(NH4)2HPO4And MnCO3And the molar ratio between them is 0.35: 0.05: 2: 3: 0.1, fully grinding and uniformly mixing, placing into a corundum crucible, placing into a high-temperature furnace, roasting at 1400 ℃ for 2 hours in a nitrogen atmosphere, and then cooling to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
The excitation spectrum of the phosphor of this embodiment is a broad spectrum, which covers the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, indicating that the phosphor of this embodiment can be effectively excited by the ultraviolet and violet chips. The phosphor of this embodiment emits blue light and red light under 360nm light excitationThe emission peaks of light and near infrared light are respectively near 450nm, 610 nm and 750nm, which shows that the fluorescent powder of the embodiment is suitable for being used as single-matrix multicolor fluorescent powder. The XRD pattern of the phosphor powder in this example shows the d value and the trend of the relative intensity change of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
Example 11
According to (Ba)0.2Mg0.2)Hf2(PO4)3：0.1Mn2+Weighing BaCO3、MgCO3、HfO2、NH4H2PO4And MnCO3And the molar ratio between them is 0.2: 0.2: 2: 3: 0.1, fully grinding and uniformly mixing, placing into a corundum crucible, placing into a high-temperature furnace, roasting at 1300 ℃ for 4 hours under the argon atmosphere, and then cooling to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
The excitation spectrum of the phosphor of this embodiment is a broad spectrum, which covers the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, indicating that the phosphor of this embodiment can be effectively excited by the ultraviolet and violet chips. Under the excitation of 360nm light, the phosphor of the embodiment emits blue light, red light and near infrared light, and the emission peaks are respectively located near 450nm, 610 nm and 750nm, which indicates that the phosphor of the embodiment is suitable for being used as single-matrix multicolor phosphor. The XRD pattern of the phosphor powder in this example shows the d value and the trend of the relative intensity change of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
Example 12
According to (Ba)0.449Mg0.05)Hf2(PO4)3：0.001Mn2+Weighing BaCO3、MgCO3、HfO2、(NH4)2HPO4And MnCO3And the molar ratio between them is 0.449: 0.05: 2: 3: 0.001, after fully grinding and uniformly mixing, placing the mixture in a corundum crucible, and then placing the corundum crucible into a high positionAnd (3) roasting in a warm furnace at 1400 ℃ for 2 hours in a nitrogen atmosphere, and then cooling to room temperature to obtain the fluorescent powder for the LED lamp for plant growth.
The excitation spectrum of the phosphor of this embodiment is a broad spectrum, which covers the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, indicating that the phosphor of this embodiment can be effectively excited by the ultraviolet and violet chips. Under the excitation of 360nm light, the phosphor of the embodiment emits blue light, red light and near infrared light, and the emission peaks are respectively located near 450nm, 610 nm and 750nm, which indicates that the phosphor of the embodiment is suitable for being used as single-matrix multicolor phosphor. The XRD pattern of the phosphor powder in this example shows the d value and the trend of the relative intensity change of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
Example 13
According to (Ba)0.299Mg0.2)Hf2(PO4)3：0.001Mn2+Weighing BaCO3、MgCO3、HfO2、NH4H2PO4And MnCO3And the molar ratio between them is 0.299: 0.2: 2: 3: 0.001, fully grinding and uniformly mixing, placing into a corundum crucible, placing into a high-temperature furnace, roasting at 1300 ℃ for 4 hours under the argon atmosphere, and then cooling to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
The excitation spectrum of the phosphor of this embodiment is a broad spectrum, which covers the ultraviolet and violet regions, and the excitation peaks are located near 300nm and 360nm, indicating that the phosphor of this embodiment can be effectively excited by the ultraviolet and violet chips. Under the excitation of 360nm light, the phosphor of the embodiment emits blue light, red light and near infrared light, and the emission peaks are respectively located near 450nm, 610 nm and 750nm, which indicates that the phosphor of the embodiment is suitable for being used as single-matrix multicolor phosphor. The XRD pattern of the phosphor powder in this example shows the d value and the trend of the relative intensity change of the product and the standard Ba0.5Zr2(PO4)3Standard card (JCPDF: 250171) was consistent, indicating that the phosphor synthesized in this example has a higher purity.
The above-described embodiments are intended to illustrate rather than to limit the invention, and any modifications and variations of the present invention are within the spirit of the invention and the scope of the appended claims.
Claims (5)
1. The fluorescent powder for the LED lamp for plant growth is characterized by having the following chemical expression: (Ba)0.5-x- yMgy)M2(PO4)3：xMn2+Wherein M is any one of Zr, Ce and Hf, x is 0.001-0.1, and y is 0.05-0.2.
2. A preparation method of fluorescent powder for a plant growth LED lamp is characterized by comprising the following steps:
(1) with barium carbonate, magnesium carbonate, M-containing oxide, [ PO ]4]3-Compound and manganese carbonate according to the chemical formula (Ba)0.5-x- yMgy)M2(PO4)3：xMn2+Wherein M is any one of Zr, Ce and Hf, x is 0.001-0.1, and y is 0.05-0.2 to obtain a mixture; (2) and putting the mixture into a crucible, sintering for 2-4 hours in a high-temperature furnace at 1300-1400 ℃ of protective atmosphere, and cooling to room temperature to obtain the fluorescent powder for the plant growth LED lamp.
3. The method for preparing phosphor for LED lamp for plant growth according to claim 2, wherein the compound containing M is any one of zirconium oxide, cerium oxide and hafnium oxide.
4. The method for preparing fluorescent powder for LED lamp for plant growth according to claim 2, wherein the fluorescent powder comprises [ PO ]4]3-The compound is one of diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
5. The method for preparing phosphor for LED lamp for plant growth according to claim 2, wherein the reducing atmosphere is nitrogen or argon.
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