CN114958348A - Nitrogen oxide blue-green light information storage luminescent material and preparation method and application thereof - Google Patents
Nitrogen oxide blue-green light information storage luminescent material and preparation method and application thereof Download PDFInfo
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- CN114958348A CN114958348A CN202210524797.XA CN202210524797A CN114958348A CN 114958348 A CN114958348 A CN 114958348A CN 202210524797 A CN202210524797 A CN 202210524797A CN 114958348 A CN114958348 A CN 114958348A
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
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Abstract
The invention belongs to the technical field of luminescent materials, and particularly relates to a nitric oxide blue-green light information storage luminescent material, and a preparation method and application thereof. The invention prepares BaSi by a high-temperature solid-phase reaction method 2 O 2 N 2 And the fluorescent enhanced nitrogen oxide blue-green light information storage luminescent material is prepared by a deposition precipitation method. The chemical general formula of the luminescent material is Ba 1‑x Si 2 O 2 N 2 :xEu 2+ Wherein x is more than 0 and less than or equal to 0.2. The luminescent material prepared by the invention has the advantages of obviously enhanced luminous intensity, high purity of synthesized target luminescent material products, excellent thermal stability and capability of better meeting the practical application requirements of high-quality white light LEDs or optical information storage.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to a nitric oxide blue-green light information storage luminescent material, and a preparation method and application thereof.
Background
Solid state lighting is one of the most promising light sources due to its high energy efficiency, ideal color rendering index, long life, environmental protection, etc. In order to obtain efficient white solid state lighting, two types of phosphor-converted white light emitting diodes have been proposed. One method is to coat the InGaN-based blue light chip with yellow light-emitting phosphor powder Y 3 Al 5 O 12 :Ce 3+ (YAG:Ce 3+ ) Blue light emitted by the blue light chip and YAG: Ce 3+ The yellow light emitted by the yellow luminescent material is mixed to form white light. However, excessive blue light is easily generated in the process, and due to lack of red light components, the white light generally shows that the color temperature is higher and cannot be adjusted, and the color rendering index is lower, so that the application of the white light in the field of illumination is greatly limited; another is to use a combination of red/green/blue phosphors in combination with ultraviolet Leds. The three-color phosphor type light emitting diode has a high color rendering index and high thermal stability, and can produce efficient WLEDs at a proper color temperature. However, the conventional oxide phosphor has some inherent disadvantages such as short excitation and emission wavelengths and poor stability. Therefore, the development of novel efficient luminescent materials capable of being excited by blue/near ultraviolet light is of great significance for white light solid-state lighting applications.
In recent years, rare earth doped nitrogen silicate fluorescent powder has received more and more attention due to its good chemical stability, high luminous efficiency, long service life and environmental friendliness. E.g. alpha/beta-SiAlON, MSi 2 O 2 N 2 (M＝Ba,Sr,Ca)，M 2 Si 5 N 8 (M＝Ba,Sr,Ca)，Ba 3 Si 6 O 12 N 2 And SrSiAlON material, has high stability and excellent luminescence property due to a large amount of crystal field splitting and scattering effects caused by the coordination environment around the activation center, and has remarkable development potential.
Wherein, BaSi 2 O 2 N 2 :Eu 2+ Has been proven to be useful as cyan light compensator in high color rendering light source applications, and has excellent persistent light emission, enabling use for optical information storage. However, using traditionsBaSi prepared by high-temperature solid-phase synthesis method 2 O 2 N 2 The basic fluorescent materials still have certain defects, unknown phases often exist in the phase composition of the synthetic luminescent materials, and the luminous intensity of the synthetic luminescent materials needs to be further improved to meet the requirements of practical application of WLEDs and optical information storage.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a nitrogen oxide blue-green light information storage luminescent material, a preparation method and application thereof, and the prepared blue-green light BaSi material has stable physical and chemical properties, excellent luminescent property and no impurity phase 2 O 2 N 2 A luminescent material.
The invention provides a preparation method of a nitrogen oxide blue-green light information storage luminescent material, which comprises the following steps:
(1) according to the chemical formula BaSi 2 O 2 N 2 The raw materials are weighed according to the stoichiometric ratio, and the weighed raw materials are respectively SiO 2 、BaCO 3 、Si 3 N 4 Grinding the weighed raw materials fully, then carrying out heat treatment in a weak reducing atmosphere, and then cooling and grinding to obtain BaSi 2 O 2 N 2 A substrate;
(2) according to the chemical formula Ba 1-x Si 2 O 2 N 2 :xEu 2+ Respectively weighing Eu in a stoichiometric ratio of 2 O 3 And BaSi prepared in the step (1) 2 O 2 N 2 X is more than 0 and less than or equal to 0.2;
(3) eu is mixed 2 O 3 Dissolving in 50ml water, adding nitric acid to adjust pH to 2, stirring thoroughly for 30min, adding ammonia water to adjust pH to 6-7, and stirring again for 30min to obtain Eu 2 O 3 Solution a with mass concentration of 0.075-0.15%;
(4) magnetically stirring the solution a at normal temperature, and adding BaSi into the solution 2 O 2 N 2 Adding ammonia water into the substrate again to adjust the pH value to be 10-11, and then centrifuging, washing and drying the substrate to prepare powder b;
(5) and (3) performing heat treatment on the powder b in a weak reducing atmosphere, and cooling along with the furnace to obtain the nitric oxide blue-green luminescent material.
In the above technical solution, further, Si in the step (1) 3 N 4 Is alpha-Si 3 N 4 。
In the above technical solution, further, the weak reducing atmosphere in the step (1) is H with a volume percentage of 3% 2 And 97% of N 2 The mixed gas of (1).
In the above technical solution, further, the heat treatment in the step (1) is calcination at 1450 ℃ for 5-10 h.
In the above technical solution, further, the flow rate of the weak reducing atmosphere in the step (1) is 50-200 ml/min.
In the above technical solution, further, the weak reducing atmosphere in the step (5) is H with a volume percentage of 3% 2 And 97% of N 2 The mixed gas of (1).
In the above technical solution, further, in the step (5), the heat treatment is calcination at 1450 ℃ for 5-10h under 800-.
In the above technical solution, further, in the step (5), the flow rate of the weak reducing atmosphere is 50 to 200 ml/min.
The invention also provides a nitrogen oxide blue-green light information storage luminescent material prepared by the preparation method, and the chemical general formula of the luminescent material is Ba 1-x Si 2 O 2 N 2 :xEu 2+ Wherein x is more than 0 and less than or equal to 0.2; the luminescent material emits blue-green light with the peak wavelength of 494nm when being excited at 250-500 nm.
In another aspect, the present invention provides an information storage method for the above nitrogen oxide blue-green light information storage luminescent material, wherein the storage method comprises the following steps:
1) recording of optical information
Placing the luminescent material into a sample cell, pressing flatly, covering a layer of photomask with target pattern information on the luminescent material, irradiating for 1-5min by using an ultraviolet lamp, and recording information of the sample coated with the photomask;
2) reading of optical information
And (3) closing the ultraviolet lamp irradiation light source and removing the photomask, observing in a dark environment until afterglow completely disappears, placing the sample cell on a heating platform, heating to the temperature of 100-.
By adopting the technical scheme, the invention has the following beneficial effects:
according to the nitrogen oxide blue-green light information storage luminescent material obtained by the invention, Eu-doped ions are distributed on the surface of the substrate in a highly dispersed manner, so that the luminescent brightness of the luminescent material is obviously improved, and under the excitation of blue light and near ultraviolet, an emission peak is positioned in 494nm color waveband and is used as a cyan light compensator, so that the color rendering index of a white light LED is improved, and the luminescent brightness higher than that of a traditional high-temperature solid-phase reaction method can be generated. The preparation method has the advantages of simple process, mature technology and good industrialization prospect and application prospect.
Drawings
FIG. 1 shows luminescent materials prepared in example 1 and comparative examples 1 to 3 and BaSi 2 O 2 N 2 The XRD spectrum of the data comparison of the PDF standard card;
FIG. 2 is an emission spectrum at an excitation wavelength of 375nm of the luminescent materials prepared in example 1 and comparative example 1;
FIG. 3 is an emission spectrum at an excitation wavelength of 375nm of luminescent materials obtained in example 1 and comparative example 2;
FIG. 4 is an emission spectrum at an excitation wavelength of 375nm of the luminescent materials prepared in example 1 and comparative example 3;
fig. 5 is a graph comparing the optical information storage effects of example 2 and comparative example 4.
Detailed Description
The invention is further illustrated with reference to the following examples, without limiting the scope of the invention thereto.
Comparative example 1
| Raw materials | Weight (g) |
| BaCO 3 | 3.868 |
| SiO 2 | 0.601 |
| Si 3 N 4 | 1.403 |
| Eu 2 O 3 | 0.070 |
The traditional synthesis process of the nitrogen oxide luminescent material is adopted:
grinding the above raw materials, mixing, placing into crucible, and placing in high temperature tube furnace at 3% H 2 +97％N 2 Calcining at 1450 deg.C for 5 hr in mixed atmosphere, and cooling to room temperature to obtain Ba 0.98 Si 2 O 2 N 2 :0.02Eu 2+ Blue-green luminescent material, denoted as (SSR-0.02).
The excitation spectrum of the nitric oxide blue-green luminescent material of the comparative example is a wide spectrum, which covers near ultraviolet, purple light and blue light regions (250-500nm), and the optimal excitation peak is positioned near 375 nm. Under the excitation of 375nm near ultraviolet light, the emission peak of the luminescent material is positioned near 494 nm.
Comparative example 2
| Raw materials | Weights (g) |
| BaCO 3 | 3.868 |
| SiO 2 | 0.601 |
| Si 3 N 4 | 1.403 |
| Eu 2 O 3 | 0.070 |
The traditional nitrogen oxide luminescent material is synthesized and then is washed by water:
grinding the above raw materials, mixing, placing into crucible, and placing in high temperature tube furnace at 3% H 2 +97％N 2 Calcining at 1450 deg.C for 5 hr in mixed atmosphere, cooling to room temperature, grinding, washing with deionized water for 1 hr, and drying to obtain Ba 0.98 Si 2 O 2 N 2 :0.02Eu 2+ Blue-green luminescent material, denoted as (SSR-0.02-w).
The excitation spectrum of the nitric oxide blue-green luminescent material of the comparative example is a wide spectrum, which covers near ultraviolet, purple light and blue light regions (250-500nm), and the optimal excitation peak is positioned near 375 nm. Under the excitation of 375nm near ultraviolet light, the emission peak of the luminescent material is positioned near 494 nm.
Comparative example 3
| Raw materials | Weights (g) |
| BaCO 3 | 3.868 |
| SiO 2 | 0.601 |
| Si 3 N 4 | 1.403 |
| Eu 2 O 3 | 0.070 |
The nitrogen oxide luminescent material synthesized by adopting a two-step high-temperature solid phase method is washed by water:
(1) firstly, according to the chemical formula BaSi 2 O 2 N 2 The stoichiometric ratio of (A) was weighed to give 3.868g of barium carbonate (BaCO) 3 ) 0.601g of silicon dioxide (SiO) 2 ) 1.403g of silicon nitride (Si) 3 N 4 ). Grinding in agate mortar, loading into crucible, and heating in high-temperature tube furnace at 3% H 2 +97％N 2 Calcining at 1450 deg.C for 5 hr in mixed atmosphere, and cooling to room temperature to obtain BaSi 2 O 2 N 2 A substrate.
(2) Secondly, the BaSi prepared above is mixed with the mixture 2 O 2 N 2 Matrix (5.07g) and 0.07g europium oxide (Eu) 2 O 3 ) Grinding, mixing, loading into crucible, and heating in high temperature tubular furnace at 3% H 2 +97％N 2 Calcining at 1450 deg.C for 5 hr in mixed atmosphere, cooling to room temperature, grinding, washing with deionized water for 1 hr, and drying to obtain Ba 0.98 Si 2 O 2 N 2 :0.02Eu 2+ Blue-green luminescent material, notation (SSR-0.02-10)h-w)。
The excitation spectrum of the nitric oxide blue-green luminescent material of the comparative example is a wide spectrum, which covers near ultraviolet, purple light and blue light regions (250-500nm), and the optimal excitation peak is positioned near 375 nm. Under the excitation of 375nm near ultraviolet light, the emission peak of the luminescent material is positioned near 494 nm.
Comparative example 4
The optical information storage process adopting the traditional nitrogen oxide luminescent material comprises the following steps:
(1) ba prepared in comparative example 1 was selected 0.98 Si 2 O 2 N 2 :0.02Eu 2+ (SSR-0.02) 2g of blue-green luminescent material;
(2) putting the selected material into a sample cell with the diameter of 15mm and the depth of 5mm, pressing the sample cell flat, and covering a layer of photomask with a 'love heart' pattern on the material;
(3) irradiating the sample coated with the 'love' pattern photomask by using an ultraviolet lamp for 3min, namely, an information input link;
(4) turning off an ultraviolet lamp irradiation light source, removing a photomask, and observing and photographing in a dark environment to record the afterglow phenomenon of the sample;
(5) and (3) after afterglow completely disappears, placing the sample on a heating platform at 150 ℃, and observing and photographing under a dark environment for recording, namely the information reading link.
Example 1
| Raw materials | Weight (g) |
| BaCO 3 | 3.868 |
| SiO 2 | 0.601 |
| Si 3 N 4 | 1.403 |
| Eu 2 O 3 | 0.070 |
A preparation method of a fluorescence-enhanced nitrogen oxide blue-green light information storage luminescent material comprises the following steps:
(1) according to the chemical formula BaSi 2 O 2 N 2 Respectively weighing 3.868g of barium carbonate (BaCO) 3 ) 0.601g of Silica (SiO) 2 ) 1.403g of silicon nitride (Si) 3 N 4 ) After being sufficiently ground in an agate mortar, the mixture is put into a crucible and put into a high-temperature tube furnace at 3% H 2 +97％N 2 Calcining at 1450 deg.C for 5 hr in mixed atmosphere, and cooling to room temperature to obtain BaSi 2 O 2 N 2 A substrate;
(2) 0.07g of europium oxide (Eu) 2 O 3 ) Dissolving in 50ml of water, fully stirring for 30min, adding nitric acid to adjust the pH to 2, adding ammonia water to adjust the pH to 6, and stirring for 30min again to obtain a solution a;
(3) magnetically stirring the solution a at normal temperature, and adding the weighed BaSi 2 O 2 N 2 Adding ammonia water into a substrate (4.076g) again to adjust the pH value to 11, centrifuging, washing and drying to prepare powder b;
(4) placing the powder b in a crucible, feeding into a high-temperature tube furnace, and reacting at 3% H 2 +97％N 2 Heat treatment is carried out for 5 hours under the condition of (volume ratio) atmosphere and 1450 ℃, and Ba is prepared after furnace cooling 0.98 Si 2 O 2 N 2 :0.02Eu 2+ A blue-green light-emitting material is referred to as (DP-0.02).
The blue-green luminescent material of nitrogen oxide in this embodiment has a broad spectrum, which covers the near ultraviolet, violet and blue regions (250-500nm), and the optimal excitation peak is located near 375 nm. Under the excitation of 375nm near ultraviolet light, the emission peak of the luminescent material is positioned near 494 nm.
Example 2
A light information storage method of a fluorescence-enhanced nitrogen oxide blue-green light information storage luminescent material comprises the following steps:
(1) ba prepared in example 1 was selected 0.98 Si 2 O 2 N 2 :0.02Eu 2+ (DP-0.02) blue-green luminescent material 2 g;
(2) putting the selected material into a sample cell with the diameter of 15mm and the depth of 5mm, pressing the sample cell flat, and covering a layer of photomask with a 'love heart' pattern on the material;
(3) irradiating the sample coated with the 'love' pattern photomask by using an ultraviolet lamp for 3min, namely, an information input link;
(4) turning off an ultraviolet lamp irradiation light source, removing a photomask, and observing and photographing in a dark environment to record the afterglow phenomenon of the sample;
(5) and (3) after the afterglow completely disappears, placing the sample on a heating platform at 150 ℃, and observing and photographing and recording in a dark environment, namely a reading link of information.
FIG. 1 shows luminescent materials prepared in example 1 and comparative examples 1 to 3 and BaSi 2 O 2 N 2 As can be seen from FIG. 1, the luminescent material DP-0.02 prepared by the present invention, and the luminescent materials SSR-0.02, SSR-0.02-w and SSR-0.02-10h-w prepared in comparative examples 1-3, and BaSi 2 O 2 N 2 The standard cards ICDD 058-0025 are consistent, and the diffraction peaks correspond to one another.
Fig. 2 shows emission spectra of the luminescent materials prepared in example 1 and comparative example 1 at an excitation wavelength of 375nm, and it can be seen from fig. 2 that the luminescent materials emit blue-green light under excitation of 375nm near ultraviolet light, and the emission peak is located near 494 nm. The process used by the invention has obvious effect on improving the luminous intensity of the luminescent material, and the luminous intensity is 2 times of that of the traditional process.
Fig. 3 is an emission spectrum at an excitation wavelength of 375nm of the luminescent materials prepared in example 1 and comparative example 2, and it can be seen from fig. 3 that the luminescent material emits blue-green light under excitation of 375nm near ultraviolet light, and the emission peak is located near 494 nm. The process used by the invention has obvious effect on improving the luminous intensity of the luminescent material, and the luminous intensity is 1.5 times of that of the traditional process.
Fig. 4 is an emission spectrum of the luminescent materials prepared in example 1 and comparative example 3 at an excitation wavelength of 375nm, and it can be seen from fig. 4 that the luminescent material emits bluish-green light under the excitation of 375nm near ultraviolet light, and an emission peak is located near 494 nm. The process used by the invention has obvious effect on improving the luminous intensity of the luminescent material, and the luminous intensity is 1.3 times of that of the traditional process.
Fig. 5 is a graph comparing the optical information storage effects of example 2 and comparative example 4, and the light emitting effect of example 2 is better than that of comparative example 4 under the excitation of near ultraviolet light, afterglow and thermal stimulation. The process used by the invention has obvious effect on improving the luminous intensity of the luminous material in optical information storage.
The above-mentioned embodiments are intended to illustrate the present invention, and the scope of the present invention should not be limited thereby, and any equivalent changes or equivalent modifications made to the present invention within the spirit of the present invention and the scope of the appended claims should fall within the scope of the present invention.
Claims (10)
1. A preparation method of nitrogen oxide blue-green light information storage luminescent material is characterized in that: the preparation method comprises the following steps:
(1) according to the chemical formula BaSi 2 O 2 N 2 The raw materials are weighed according to the stoichiometric ratio, and the weighed raw materials are respectively SiO 2 、BaCO 3 、Si 3 N 4 The weighed raw materials are fully ground and then are subjected to heat treatment in a weak reducing atmosphere, and then are cooled and ground to obtain BaSi 2 O 2 N 2 A substrate;
(2) according to the chemical formula Ba 1-x Si 2 O 2 N 2 :xEu 2+ Respectively weighing Eu in a stoichiometric ratio of 2 O 3 And Ba prepared in step (1)Si 2 O 2 N 2 X is more than 0 and less than or equal to 0.2;
(3) eu is mixed 2 O 3 Dissolving in 50ml water, adding nitric acid to adjust pH to 2, stirring thoroughly for 30min, adding ammonia water to adjust pH to 6-7, stirring again for 30min to obtain Eu 2 O 3 Solution a with mass concentration of 0.075-0.15%;
(4) magnetically stirring the solution a at normal temperature, and adding BaSi into the solution 2 O 2 N 2 Adding ammonia water into the substrate again to adjust the pH value to be 10-11, and then centrifuging, washing and drying the substrate to prepare powder b;
(5) and (3) performing heat treatment on the powder b in a weak reducing atmosphere, and cooling along with the furnace to obtain the nitric oxide blue-green luminescent material.
2. The method of claim 1, wherein: si in the step (1) 3 N 4 Is alpha-Si 3 N 4 。
3. The method of claim 1, wherein: the weak reducing atmosphere in the step (1) is H with the volume percentage of 3 percent 2 And 97% of N 2 The mixed gas of (1).
4. The method of claim 1, wherein: the heat treatment in the step (1) is calcination at the temperature of between 800 and 1450 ℃ for 5 to 10 hours.
5. The method of claim 1, wherein: the flow rate of the weak reducing atmosphere in the step (1) is 50-200 ml/min.
6. The method of claim 1, wherein: the weak reducing atmosphere in the step (5) is H with the volume percentage of 3 percent 2 And 97% of N 2 The mixed gas of (1).
7. The method for preparing the fluorescence-enhanced nitrogen oxide blue-green light information storage luminescent material according to claim 1, wherein the method comprises the following steps: in the step (5), the heat treatment is carried out for 5-10h under the conditions of 800-1450 ℃.
8. The method of claim 1, wherein: in the step (5), the flow rate of the weak reducing atmosphere is 50-200 ml/min.
9. The nitrogen oxide blue-green light information storage luminescent material prepared by the preparation method of any one of claims 1 to 8, wherein the chemical general formula of the luminescent material is Ba 1-x Si 2 O 2 N 2 :xEu 2+ Wherein x is more than 0 and less than or equal to 0.2; the luminescent material emits blue-green light with the peak wavelength of 494nm when being excited at 250-500 nm.
10. An information storage method of the nitrogen oxide blue-green light information storage luminescent material as claimed in claim 9, wherein the storage method comprises the steps of:
1) recording of optical information
Placing the luminescent material into a sample cell, pressing flatly, covering a layer of photomask with target pattern information on the luminescent material, irradiating for 1-5min by using an ultraviolet lamp, and recording information of the sample coated with the photomask;
2) reading of optical information
And (3) closing the ultraviolet lamp irradiation light source and removing the photomask, observing in a dark environment until afterglow completely disappears, placing the sample cell on a heating platform, heating to the temperature of 100-.
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2022
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