CN113861968B - Cr-doped 3+ Near infrared nano fluorescent powder as well as preparation method and application thereof - Google Patents
Cr-doped 3+ Near infrared nano fluorescent powder as well as preparation method and application thereof Download PDFInfo
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- CN113861968B CN113861968B CN202111262452.3A CN202111262452A CN113861968B CN 113861968 B CN113861968 B CN 113861968B CN 202111262452 A CN202111262452 A CN 202111262452A CN 113861968 B CN113861968 B CN 113861968B
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Abstract
The invention provides a Cr-doped alloy 3+ The chemical expression of the near infrared nano fluorescent powder is as follows: ga 2‑X O 3 :xCr 3+ Wherein x is more than 0 and less than 0.5, the fluorescent powder prepared by the preparation method is nano particles, is easy to dope matrix materials, and realizes the efficient conversion from blue-violet light to near infrared light; the strongest excitation peak of the fluorescent powder is highly coupled with the strongest emission peak of the GaN LED, so that the fluorescent powder can realize the efficient emission of near infrared light under the excitation of blue-violet light of a GaN LED chip, is highly matched with the requirement of a fresh-keeping spoilage detection system light source, and can be applied to the field of fresh-keeping nondestructive detection.
Description
Technical Field
The invention relates to the technical field of luminescent materials, in particular to a Cr-doped luminescent material 3+ Near infrared nano fluorescent powder, a preparation method and application thereof.
Background
Fruits and vegetables provide abundant vitamins and various minerals for human bodies, and are an important source of nutrient intake indispensable in daily life of people. Fruits and vegetables belong to fresh products, are not easy to preserve, are easy to damage and rot and grow bacteria, and people eat the deteriorated fruits and vegetables easily to cause health problems. Therefore, a method for rapidly judging the quality of fresh products is needed.
In recent years, spectroscopic techniques have been widely used in the field of food detection. The near infrared spectrum technology is mainly used for absorbing electromagnetic waves in the wavelength range of 700-1500nm by using molecular vibration of a plant organism to obtain image differences of normal and spoiled organisms, and is a method capable of rapidly judging the quality of fresh products and a nondestructive detection technology with very good application prospects.
At present, light sources for providing near infrared light are various, such as an infrared LED chip, an epitaxial heterojunction thin film light source and the like, wherein the emission spectrum of the infrared LED chip is narrow, and the application is limited; although the epitaxial heterojunction thin film light source has better near infrared fluorescence emission, the manufacture of the epitaxial heterojunction thin film light source requires precise and expensive equipment such as chemical vapor deposition, molecular beam epitaxy and the like, and also requires expensive and unstable organometallic precursors such as Cd, hg, pb and the like, and the manufacture cost is high.
Compared with the traditional light source, the fluorescent light of the blue-violet LED chip can be efficiently converted into near-infrared fluorescent light by introducing the activating agent into the matrix material, so that the fluorescent light source is a near-infrared light source with application potential. Wherein Cr is used 3+ Luminescent materials made by doping borates, silicates and aluminates as activators have wide absorption/excitation bands and excellent spectral reactions, and are important targets for exploration. However, such Cr 3+ The doped fluorescent powder needs to be subjected to solid phase reaction for 5-10 hours at the high temperature of 700-1500 ℃ during preparation, and is time-consuming and energy-consuming; the prepared luminescent material is in a micro-millimeter level, is large in size and not easy to be uniformly doped, is not beneficial to packaging and propagation of ultraviolet excitation light, and affects the conversion efficiency of near infrared light.
Disclosure of Invention
The invention aims to provide a Cr-doped alloy 3+ The near infrared nano fluorescent powder is in nano level and small in size, is beneficial to doping, packaging and propagation of ultraviolet excitation light, and improves the conversion efficiency of infrared light; meanwhile, the preparation method greatly reduces the calcining temperature and time and has low energy consumption.
One aspect of the invention provides a Cr-doped alloy 3+ Is of (3)Fluorescent powder with chemical expression of Ga 2-X O 3 :xCr 3+ Wherein x is more than 0 and less than 0.5, the fluorescent powder is nano particles, and the average particle size is 5-100nm.
Another aspect of the invention provides the above-described doped Cr 3+ The preparation method of the near infrared nano fluorescent powder comprises the following steps:
s1, ga according to chemical expression 2-X O 3 :xCr 3+ The stoichiometric ratio of each chemical component in the mixture is respectively weighed Ga 3+ Raw material, cr 3+ Raw materials, OH - Mixing the raw materials with a molten salt protective agent;
s2, adding ethanol or water into the mixture obtained in the step S1, and grinding uniformly;
s3, vacuum drying the mixture obtained in the step S2;
s4, transferring the mixture obtained in the step S3 into an alumina crucible, and calcining;
and S5, cooling the mixture obtained in the step S4 to room temperature, washing, drying and grinding to obtain the nano fluorescent powder.
Further, in the step S4, the calcination temperature is 200-500 ℃ and the calcination time is 1-5 hours.
Further, in the step S4, the calcination temperature is 300 ℃ and the calcination time is 2 hours.
Further, in the S1 step, ga 3+ The raw material is Ga (NO) 3 ) 3 Or GaCl 3 ；Cr 3+ The raw material is Cr (NO) 3 ) 3 Or CrCl 3 ；OH - The raw materials are ammonia water, sodium hydroxide or potassium hydroxide; the molten salt protecting agent is sodium chloride or potassium chloride.
Further, the fluorescent powder prepared by the method has excitation wavelength in a range of 250-680nm and 3 excitation peaks, the emission wavelength of the fluorescent powder is in a range of 650-1100nm, and the strongest excitation peak of the fluorescent powder is highly coupled with the strongest emission peak of the GaN LED. The high-efficiency emission of near infrared light can be realized under the excitation of blue-violet light of the GaN LED chip, the high-efficiency emission is highly matched with the requirements of fresh and putrefactive detection light sources, and the high-efficiency detection light source can be applied to the field of fresh and nondestructive detection.
The beneficial effects of the invention are as follows:
the invention provides the doped Cr 3+ The near infrared nano fluorescent powder is in nano level, has small size, is favorable for packaging and spreading ultraviolet excitation light, and improves the conversion efficiency of infrared light.
The invention provides the doped Cr 3+ The preparation method of the near infrared nano fluorescent powder is simple and is easy for industrial production. Compared with the prior art, the method greatly reduces the calcining temperature and time, saves energy consumption, has low requirements on preparation equipment and conditions, and effectively reduces the preparation cost; in addition, the preparation method has the advantages of wide sources of raw materials, low price, environmental friendliness and no pollutant in the preparation process; the fluorescent powder prepared by the preparation method does not need a metal precursor, and the preparation cost is further reduced.
The invention provides the doped Cr 3+ The near infrared nano fluorescent powder has excitation wavelength in 250-680nm range and emission wavelength in 650-1100nm range, has wider excitation band and emission band, and provides a wide-band near infrared luminescent material, so that the near infrared nano fluorescent powder is applied to the infrared detection field.
The invention provides the doped Cr 3+ The near infrared nano fluorescent powder can realize high-efficiency emission of near infrared light under the excitation of blue-violet light of an LED chip, is highly matched with the light source requirement of fruit and vegetable spoilage detection, and can be applied to the detection of the quality of fresh products.
Drawings
FIG. 1 is a photograph of a phosphor according to a sixth embodiment of the present invention.
FIG. 2 is a transmission electron micrograph of a phosphor according to a sixth embodiment of the present invention.
FIG. 3 is an X-ray diffraction chart of a phosphor in a sixth embodiment of the present invention.
FIG. 4 is a graph showing the excitation and emission spectra of a phosphor according to a sixth embodiment of the present invention.
Detailed Description
So that the manner in which the above recited objects, features and advantages of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to embodiments, some of which are illustrated in the appended drawings.
Embodiment one:
s1, selecting Ga (NO) 3 ) 3 、CrCl 3 Sodium hydroxide, sodium chloride and water are used as raw materials, and Ga is expressed according to fluorescence powder chemistry 2-X O 3 :xCr 3+ The stoichiometric ratio of each chemical component in the mixture was 1.99mmol Ga (NO) 3 ) 3 、0.01mmol CrCl 3 Mixing 1mmol of sodium hydroxide and 2mmol of sodium chloride raw materials;
s2, adding 5mL of water into the mixture obtained in the step S1, grinding for 15 minutes, and uniformly mixing;
s3, vacuum drying the mixture obtained in the step S2 for 20 minutes;
s4, transferring the powder obtained in the step S3 into an alumina crucible, placing the alumina crucible into a box-type furnace, and calcining at 200 ℃ for 1 hour;
s5, after the mixture obtained in the step S4 is cooled to room temperature, washing, drying and grinding to obtain Ga 1.99 O 3 :0.01Cr 3+ Nano fluorescent powder.
Embodiment two:
s1, selecting Ga (NO) 3 ) 3 、CrCl 3 Sodium hydroxide, sodium chloride and water are used as raw materials, and Ga is expressed according to fluorescence powder chemistry 2-X O 3 :xCr 3+ The stoichiometric ratio of each chemical component in the mixture was measured, 1.6mmol Ga (NO) 3 ) 3 、0.4mmol CrCl 3 Mixing 2mmol of sodium hydroxide and 8mmol of sodium chloride raw materials;
s2, pouring the mixture obtained in the step S1 into 10mL of water, grinding for 15 minutes, and uniformly mixing;
s3, vacuum drying the mixture obtained in the step S2 for 20 minutes;
s4, transferring the powder obtained in the step S3 into an alumina crucible, placing the alumina crucible into a box-type furnace, and calcining at 500 ℃ for 5 hours;
s5, after the mixture obtained in the step S4 is cooled to room temperature, washing, drying and grinding to obtain Ga 1.6 O 3 :0.4Cr 3 + Nano fluorescent powder.
Embodiment III:
s1, selecting GaCl 3 、Cr(NO 3 ) 3 Potassium hydroxide, potassium chloride and ethanol are used as raw materials, and Ga is expressed according to fluorescence powder chemistry 2-X O 3 :xCr 3+ The stoichiometric ratio of each chemical component in the mixture was measured, 1.55mmol Ga (NO) 3 ) 3 、0.45mmol CrCl 3 Mixing 1.5mmol of potassium hydroxide and 10mmol of potassium chloride raw materials;
s2, pouring the mixture obtained in the step S1 into 10mL of ethanol, grinding for 20 minutes, and uniformly mixing;
s3, vacuum drying the mixture obtained in the step S2 for 15 minutes;
s4, transferring the powder obtained in the step S3 into an alumina crucible, placing the alumina crucible into a box-type furnace, and calcining for 3 hours at 300 ℃;
s5, after the mixture obtained in the step S4 is cooled to room temperature, washing, drying and grinding to obtain Ga 1.55 O 3 :0.45Cr 3+ Nano fluorescent powder.
Embodiment four:
s1, selecting GaCl 3 、Cr(NO 3 ) 3 Potassium hydroxide, potassium chloride and ethanol are used as raw materials, and Ga is expressed according to fluorescence powder chemistry 2-X O 3 :xCr 3+ The stoichiometric ratio of each chemical component in the mixture was 1.95mmol Ga (NO) 3 ) 3 、0.05mmol CrCl 3 Mixing 1.2mmol of potassium hydroxide and 5mmol of potassium chloride raw materials;
s2, pouring the mixture obtained in the step S1 into 10mL of ethanol, grinding for 20 minutes, and uniformly mixing;
s3, vacuum drying the mixture obtained in the step S2 for 10 minutes;
s4, transferring the powder obtained in the step S3 into an alumina crucible, placing the alumina crucible into a box-type furnace, and calcining at 200 ℃ for 3 hours;
s5, after the mixture obtained in the step S4 is cooled to room temperature, washing, drying and grinding to obtain Ga 1.95 O 3 :0.05Cr 3+ Nano fluorescent powder.
Fifth embodiment:
s1, selecting GaCl 3 、Cr(NO 3 ) 3 Potassium hydroxide, potassium chloride and ethanol are used as raw materials, and Ga is expressed according to fluorescence powder chemistry 2-X O 3 :xCr 3+ The stoichiometric ratio of each chemical component in the mixture was 1.75mmol Ga (NO) 3 ) 3 、0.25mmol CrCl 3 Mixing 1.8mmol of potassium hydroxide and 8mmol of potassium chloride raw materials;
s2, pouring the mixture obtained in the step S1 into 8mL of ethanol, grinding for 20 minutes, and uniformly mixing;
s3, vacuum drying the mixture obtained in the step S2 for 10 minutes;
s4, transferring the powder obtained in the step S3 into an alumina crucible, placing the alumina crucible into a box-type furnace, and calcining at 300 ℃ for 2 hours;
s5, after the mixture obtained in the step S4 is cooled to room temperature, washing, drying and grinding to obtain Ga 1.75 O 3 :0.25Cr 3+ Nano fluorescent powder.
Example six:
s1, selecting GaCl 3 、Cr(NO 3 ) 3 Potassium hydroxide, potassium chloride and ethanol are used as raw materials, and Ga is expressed according to fluorescence powder chemistry 2-X O 3 :xCr 3+ The stoichiometric ratio of each chemical component in the mixture was measured, 1.9mmol Ga (NO) 3 ) 3 、0.1mmol CrCl 3 Mixing 1.5mmol of potassium hydroxide and 5mmol of potassium chloride raw materials;
s2, pouring the mixture obtained in the step S1 into 5mL of ethanol, grinding for 15 minutes, and uniformly mixing;
s3, vacuum drying the mixture obtained in the step S2 for 10 minutes;
s4, transferring the powder obtained in the step S3 into an alumina crucible, placing the alumina crucible into a box-type furnace, and calcining at 500 ℃ for 2 hours;
s5, after the mixture obtained in the step S4 is cooled to room temperature, washing, drying and grinding to obtain Ga 1.9 O 3 :0.1Cr 3 + Nano fluorescent powder.
FIGS. 1 and 2 show Ga obtained in accordance with a sixth embodiment of the present invention 1.9 O 3 :0.1Cr 3+ The powder picture and projection electron microscope picture of the fluorescent powder can be observed that the obtained fluorescent powder has uniform particles and the average particle diameter is about 20 nm.
FIG. 3 shows Ga according to the sixth embodiment of the present invention 1.9 O 3 :0.1Cr 3+ The X-ray diffraction pattern of the fluorescent powder can be seen from the figure, and the pattern is matched with JCPDS 41-1103 (beta-Ga 2 O 3 ) Consistent, prove successful in obtaining Ga 1.9 O 3 :0.1Cr 3+ The fluorescent powder has obvious broadening of diffraction peaks, which indicates that the fluorescent powder nano powder has better purity and no impurity phase.
FIG. 4 shows Ga according to the sixth embodiment of the present invention 1.9 O 3 :0.1Cr 3+ As can be seen from the graph, the fluorescent powder obtained in the sixth embodiment has an obvious wide excitation band in the interval of 250-680nm, and 3 excitation peaks respectively exist at 290nm, 443nm and 600 nm; the obvious wide emission band exists in the range of 650-1100nm, the emission reaches the highest at 795nm, the emission spectrum range of the GaN LED is in the range of 400-500nm, the emission center of blue-violet light is in the range of 450nm, the blue-violet light is highly coupled with the strongest excitation peak of the fluorescent powder obtained in the sixth embodiment, and the blue-violet light emission of the GaN LED can efficiently excite the near infrared fluorescence emission of the fluorescent powder. The emission spectrum of the fluorescent powder is highly matched with the light source requirement of fruit and vegetable spoilage detection, and can be pertinently applied to the field of nondestructive detection of fresh products.
Although the present disclosure is described above, the scope of protection of the present disclosure is not limited thereto. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the disclosure, and these changes and modifications will fall within the scope of the invention.
Claims (5)
1. Cr-doped 3+ The preparation method of the near infrared nano fluorescent powder is characterized by comprising the following steps:
s1, ga according to chemical expression 2-X O 3 :xCr 3+ Each chemical component of (a)Stoichiometric ratios separately weigh Ga 3+ Raw material, cr 3+ Raw materials, OH - Mixing the raw materials with a molten salt protective agent;
s2, adding the mixture obtained in the step S1 into ethanol or water, and grinding uniformly;
s3, vacuum drying the mixture obtained in the step S2;
s4, transferring the mixture obtained in the step S3 into an alumina crucible, and calcining;
s5, cooling the mixture obtained in the step S4 to room temperature, and washing, drying and grinding to obtain nano fluorescent powder;
the chemical expression of the fluorescent powder is as follows: ga 2-X O 3 :xCr 3+ Wherein x is more than 0 and less than 0.5, the fluorescent powder is nano particles, and the average particle size is 5-100nm;
in the step S4, the calcination temperature is 200-500 ℃ and the calcination time is 1-2 hours;
the molten salt protecting agent is sodium chloride or potassium chloride.
2. The method of producing phosphor according to claim 1, wherein the calcination temperature is 300 ℃ and the calcination time is 2 hours.
3. The method of producing phosphor according to claim 2, wherein the Ga 3+ The raw material is Ga (NO) 3 ) 3 Or GaCl 3 。
4. The method of claim 3, wherein the Cr 3+ The raw material is Cr (NO) 3 ) 3 Or CrCl 3 。
5. The method of producing phosphor according to claim 4, wherein said OH - The raw materials are ammonia water, sodium hydroxide or potassium hydroxide.
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Non-Patent Citations (1)
| Title |
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| 郑有炓 等.《中国战略性新星产业——新材料 第三代半导体材料》.中国铁道出版社,2017,(第1版),第212页. * |
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