CN113214821B - Application of phenolic compound in improving humidity resistance of tetravalent manganese fluoride red fluorescent powder - Google Patents
Application of phenolic compound in improving humidity resistance of tetravalent manganese fluoride red fluorescent powder Download PDFInfo
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- CN113214821B CN113214821B CN202110342404.9A CN202110342404A CN113214821B CN 113214821 B CN113214821 B CN 113214821B CN 202110342404 A CN202110342404 A CN 202110342404A CN 113214821 B CN113214821 B CN 113214821B
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/61—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing fluorine, chlorine, bromine, iodine or unspecified halogen elements
- C09K11/617—Silicates
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- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
The invention discloses an application of a phenolic compound in improving the humidity resistance of tetravalent manganese fluoride red fluorescent powder, wherein the phenolic compound is selected from one or more of hydroquinone, phloroglucinol and bisphenol A, and the mass ratio of the tetravalent manganese fluoride red fluorescent powder to the phenolic compound is 1000: (5-50), in the invention, the phenolic compound with higher melting point and moderate reducibility can reduce the hydrolysis product of tan light-absorbing manganese generated by hydrolyzing the surface of the tetravalent manganese fluoride fluorescent powder from quadrivalence to a non-light-absorbing divalent manganese compound; meanwhile, the fluoride fluorescent powder matrix can be slightly dissolved in water, after the matrix is dissolved, the doped manganese is precipitated and reduced to be consumed, and the matrix is re-deposited on the surface, so that a core-shell structure with the fluoride containing the doped manganese as a core and the fluoride without the doped manganese as a shell, namely a KXFM @ KXF structure, can prevent water from continuously hydrolyzing the fluorescent powder, and the waterproof performance of the quadrivalent manganese fluoride red fluorescent powder is improved while almost no luminescent performance loss is caused.
Description
Technical Field
The invention relates to the technical field of inorganic luminescent materials, in particular to application of a phenolic compound in improving the humidity resistance of tetravalent manganese fluoride red fluorescent powder.
Background
As lighting needs consume about 19% of the world's power, the development of new generation lighting devices has attracted increasing attention worldwide. Since Akasaki, amano and Nakamura based on InGaN blue LED inventions, the artificial lighting industry began a new era, and they consequently won the 2014 nobel prize in physics. Light Emitting Diodes (LEDs) have excellent functions such as low power consumption, compactness, light emitting efficiency and environmental friendliness, and thus are considered as potential alternatives to conventional lighting. The blue LED is mixed with yellow phosphor (Y) by a simple and inexpensive process 3 Al 5 O 12 ：Ce 3+ (YAG: ce)) combination may produce white light. However, due to the lack of red spectral region, YAG-based: the white LED of Ce shows a lower Color Rendering Index (CRI)<80 And higher correlated color temperature (CCT = 4000)8000K), which limits their applications. In order to produce warm white LEDs with high CRI values of 90 and low CCT values of 2700 to 4000K, various red phosphors are widely used (rare earth activated sulfides, tungstates, nitrides, etc.). More recently, a new type of fluoride phosphor, namely A 2 MF 6 ：Mn 4+ (A = K, na and Cs; M = Si, zr and Ti) as a red phosphor, has attracted much attention due to its excellent light emitting characteristics (including narrow-band emission), high light emitting efficiency, low thermal quenching at high temperature and high color rendering index. However, despite their many advantages, there are still key problems for commercial applications. I.e., when exposed to high humidity environments, due to the inclusion of alkaline earth metals and halide elements (e.g., na) + ，K + And F - ) The phosphor powder inside is easily affected with moisture, and the luminous efficiency is remarkably reduced.
Various coating methods have been proposed to improve the long-term stability of LED devices. In general, coating the surface of the phosphor with a hydrophobic material can make the phosphor more water-resistant under high humidity conditions. For example, a Chinese patent with publication number "CN110343518A" published as 2019, 10 and 18 discloses a phosphor coated with a heterogeneous inorganic material, wherein an inorganic inert outer layer resists water erosion. However, the fluorescent powder is coated by the hydrophobic material to prevent water, so that the luminous efficiency of the fluorescent powder is reduced. Therefore, it is highly desirable to provide a new method for improving the waterproof performance of the tetravalent manganese fluoride red phosphor.
Disclosure of Invention
The invention aims to overcome the problem that the luminous efficiency of tetravalent manganese fluoride red fluorescent powder is reduced by realizing water resistance of the tetravalent manganese fluoride red fluorescent powder through a hydrophobic material, and provides the application of a phenolic compound in improving the humidity resistance of the tetravalent manganese fluoride red fluorescent powder.
The above object of the present invention is achieved by the following technical solutions:
the application of a phenolic compound in improving the humidity resistance of tetravalent manganese fluoride red fluorescent powder is characterized in that the phenolic compound is selected from one or more of hydroquinone, phloroglucinol and bisphenol A; the mass ratio of the tetravalent manganese fluoride red fluorescent powder to the phenolic compound is 1000: (5 to 50).
The hydroquinone, the phloroglucinol and the bisphenol A have moderate reducibility and higher melting point, and can reduce a hydrolysate of tan light-absorbing manganese generated by hydrolyzing the surface of the tetravalent manganese fluoride fluorescent powder into a non-light-absorbing divalent manganese compound from quadrivalence, thereby achieving the waterproof effect. On the other hand, the fluoride fluorescent powder matrix can be slightly dissolved in water, after the matrix is dissolved, the doped manganese is precipitated and reduced to be consumed, and the matrix is deposited on the surface again, so that a core-shell structure with the fluoride containing the doped manganese as a core and the fluoride without the doped manganese as a shell, namely a KXFM @ KXF structure, is formed, and the continuous hydrolysis of water to the fluorescent powder can be prevented.
Preferably, the method for improving the moisture resistance of the tetravalent manganese fluoride red fluorescent powder by the phenolic compound comprises the following steps:
dissolving a phenolic compound in an organic solvent, adding tetravalent manganese fluoride red fluorescent powder, and performing ultrasonic drying.
Preferably, the method for improving the moisture resistance of the tetravalent manganese fluoride red fluorescent powder by the phenolic compound comprises the following steps:
grinding the phenolic compound into powder with the particle size of less than 5 mu m, adding tetravalent manganese fluoride red fluorescent powder, and uniformly mixing.
Preferably, the mass ratio of the tetravalent manganese fluoride red fluorescent powder to the phenolic compound is 1000: (5-25). More preferably 1000: (5-10).
In the present invention, the solvent may be selected from conventional solvents that can dissolve phenolic compounds. Preferably, the organic solvent is selected from one or more of ethyl ether, ethyl acetate and ethanol. Ethanol is more preferred.
Preferably, 200-800 mg of tetravalent manganese fluoride red fluorescent powder is added into each milliliter of organic solvent. More preferably, 200-500 mg of tetravalent manganese fluoride red fluorescent powder is added into each milliliter of organic solvent.
Preferably, the drying temperature is 40 to 80 ℃.
The tetravalent manganese fluoride red fluorescent powder is selected from tetravalent manganese doped fluoride fluorescent powder which is conventional in the field. Preferably, the tetravalent manganese fluoride red phosphor is tetravalent manganese-doped potassium hexafluorosilicate or tetravalent manganese-doped potassium hexafluorogermanate.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides an application of a phenolic compound in improving the humidity resistance of tetravalent manganese fluoride red fluorescent powder, in the invention, the phenolic compound with higher melting point and moderate reducibility can reduce a brownish light-absorbing manganese hydrolysate generated by hydrolyzing the surface of tetravalent manganese fluoride fluorescent powder from quadrivalence to a non-light-absorbing divalent manganese compound; meanwhile, the fluoride fluorescent powder matrix can be slightly dissolved in water, after the matrix is dissolved, the doped manganese is precipitated and reduced to be consumed, and the matrix is re-deposited on the surface, so that a core-shell structure with the fluoride containing the doped manganese as a core and the fluoride without the doped manganese as a shell, namely a KXFM @ KXF structure, can prevent water from continuously hydrolyzing the fluorescent powder, and the waterproof performance of the quadrivalent manganese fluoride red fluorescent powder is improved while almost no luminescent performance loss is caused.
Drawings
FIG. 1 is an SEM image of modified tetravalent manganese doped potassium hexafluorosilicate (KSF-HQ) and unmodified tetravalent manganese doped potassium hexafluorosilicate (KSF) prepared in example 1.
FIG. 2 is a diagram showing the state of the modified tetravalent manganese-doped potassium hexafluorosilicate (right) and the unmodified tetravalent manganese-doped potassium hexafluorosilicate (left) prepared in example 1 after being soaked in water for 24 hours under natural light irradiation.
FIG. 3 is a graph of the modified tetravalent manganese-doped potassium hexafluorosilicate (right) prepared in example 1 and the unmodified tetravalent manganese-doped potassium hexafluorosilicate (left) after soaking in water for 24h under 365nm UV lamp irradiation.
FIG. 4 is a graph showing the luminescence intensity of the modified tetravalent manganese-doped potassium hexafluorosilicate (KSF-HQ) prepared in example 1 after different soaking times than that of the unmodified tetravalent manganese-doped potassium hexafluorosilicate (KSF).
FIG. 5 is a graph of 460nm excited states of different phenol modified tetravalent manganese doped hexafluoro-silicon potassium and unmodified tetravalent manganese doped hexafluoro-silicon potassium after water immersion for 7 days.
Detailed Description
In order to more clearly and completely describe the technical scheme of the invention, the invention is further described in detail by the specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the invention, and are not used for limiting the invention, and various changes can be made within the scope defined by the claims of the invention.
The examples and comparative examples treat tetravalent manganese fluoride red phosphor by one of the following methods, including the steps of:
dissolving a phenolic compound in an organic solvent, adding tetravalent manganese fluoride red fluorescent powder, and performing ultrasonic drying;
or grinding the phenolic compound into powder with the particle size less than 5 mu m, adding tetravalent manganese fluoride red fluorescent powder, and uniformly mixing.
Example 1
This example provides the application of hydroquinone in improving the humidity resistance of tetravalent manganese fluoride red phosphor.
The method for improving the moisture resistance of the tetravalent manganese fluoride red fluorescent powder by hydroquinone comprises the following steps:
5mg of hydroquinone is dissolved in 2mL of ethanol, 1g of KSF (tetravalent manganese doped potassium hexafluorosilicate) is added, and the mixture is placed into an ultrasonic instrument to be subjected to ultrasonic treatment at 60 ℃ until the mixture is dried, so that hydroquinone-loaded KSF is obtained.
Example 2
This example is a second example of the present invention, and is different from example 1 in that the effect of phloroglucinol on the humidity resistance of tetravalent manganese fluoride red phosphor was investigated.
Example 3
This example is a third example of the present invention, and unlike example 1, this example investigated the effect of bisphenol a on the humidity resistance of tetravalent manganese fluoride red phosphor.
Example 4
This example is a fourth example of the present invention, and is different from example 1 in that the present example studies the effect of hydroquinone on the moisture resistance of KGF (tetravalent manganese doped potassium hexafluorogermanate).
Example 5
This example is a fifth example of the present invention, and unlike example 2, the present example investigates the effect of phloroglucinol on the moisture resistance of KGF.
Example 6
This example is a sixth example of the present invention, and unlike example 3, the present example investigates the effect of bisphenol a on the moisture resistance of KGF.
Example 7
This example provides the application of hydroquinone in improving the humidity resistance of tetravalent manganese fluoride red phosphor.
The method for improving the moisture resistance of the tetravalent manganese fluoride red fluorescent powder by hydroquinone comprises the following steps:
grinding 5mg of hydroquinone into powder with the particle size of less than 5 mu m, then putting the powder and 1g of KSF into the same container, and fully and uniformly mixing the powder and the KSF in a shaking way to obtain the hydroquinone-loaded KSF.
Example 8
This example is an eighth example of the present invention, and is different from example 7 in that the effect of phloroglucinol on the humidity resistance of tetravalent manganese fluoride red phosphor was investigated.
Example 9
This example is a ninth example of the present invention, and is different from example 7 in that the present example studies the influence of the moisture resistance of the red phosphor of tetravalent manganese fluoride of bisphenol a.
Example 10
This example is a tenth example of the present invention, and unlike example 7, the present example investigates the effect of hydroquinone on the moisture resistance of KGF.
Example 11
This example is an eleventh example of the present invention, which is different from example 8 in that the effect of phloroglucinol on the moisture resistance of KGF was investigated.
Example 12
This example is a twelfth example of the present invention, which is different from example 9 in that the effect of bisphenol A on the moisture resistance of KGF was investigated.
Example 13
This example is a thirteenth example of the present invention, and is different from example 1 in that this example studies the effect of 10mg of hydroquinone on the humidity resistance of tetravalent manganese fluoride red phosphor.
Example 14
This example is a fourteenth example of the present invention, and is different from example 1 in that this example studies the effect of 25mg of hydroquinone on the humidity resistance of tetravalent manganese fluoride red phosphor.
Example 15
This example is a fifteenth embodiment of the present invention, and is different from example 1 in that this example studies the influence of 50mg of hydroquinone on the humidity resistance of tetravalent manganese fluoride red phosphor.
Example 16
This example is a sixteenth example of the present invention and, unlike example 1, this example investigates the effect of 5mg hydroquinone on the moisture resistance of 1.6g KSF.
Example 17
This example is a seventeenth example of the present invention, and unlike example 1, this example investigated the effect of 5mg hydroquinone on the moisture resistance of 0.4g KSF.
Comparative example 1
This comparative example is the first comparative example of the present invention, and unlike example 1, this comparative example investigated the effect of hydroquinone below 5mg on the humidity resistance of tetravalent manganese fluoride red phosphor. Due to the shortage of hydroquinone, the phosphor powder obtained by the comparative example has poor waterproof performance.
Comparative example 2
This comparative example is the first comparative example of the present invention, and unlike example 1, this comparative example investigated the effect of hydroquinone above 50mg on the humidity resistance of tetravalent manganese fluoride red phosphor. And the luminescent property of the obtained fluorescent powder is reduced due to excessive hydroquinone.
Comparative example 3
This comparative example is a third comparative example of the present invention, and unlike example 7, this comparative example investigated the effect of hydroquinone particle size larger than 5 μm on the moisture resistance of tetravalent manganese fluoride red phosphor. The phosphor powder obtained by the comparative example has poor waterproof performance because the hydroquinone has overlarge particle size and less surface adsorption.
Comparative example 4
This comparative example is a fourth comparative example of the present invention, and unlike example 1, this comparative example investigated the effect of bisphenol fluorene on the humidity resistance of tetravalent manganese fluoride red phosphor.
Comparative example 5
This comparative example is a fifth comparative example of the present invention and unlike example 1, this comparative example investigated the effect of 1,5-dihydroxynaphthalene tetravalent manganese fluoride red phosphor on moisture resistance.
Characterization of the test
FIG. 1 is an SEM image of modified tetravalent manganese doped potassium hexafluorosilicate (KSF-HQ) and unmodified tetravalent manganese doped potassium hexafluorosilicate (KSF) prepared in example 1. As can be seen from the figure, the KSF surface is very smooth, while the KSF-HQ surface is rough, indicating successful surface loading of tetravalent manganese-doped potassium hexafluorosilicate with a layer of hydroquinone. The SEM images of the phosphors obtained in examples 2 to 17 were similar to those of KSF-HQ, and the surface phenolic compounds were observed.
2 parts of 100mg of KSF and KSF-HQ from example 1 were prepared, 1ml of each water was added, the water was poured off over 24h and then dried. Thus obtaining the KSF and the KSF-HQ which are soaked in water for 24 hours.
FIG. 2 is a diagram showing the state of the modified tetravalent manganese-doped potassium hexafluorosilicate (right) and the unmodified tetravalent manganese-doped potassium hexafluorosilicate (left) prepared in example 1 after being soaked in water for 24 hours under natural light irradiation. FIG. 3 is a graph of the modified tetravalent manganese-doped potassium hexafluorosilicate (right) and the unmodified tetravalent manganese-doped potassium hexafluorosilicate (left) prepared in example 1 after soaking in water for 24h under 365nm UV light. As can be seen from FIGS. 2 and 3, when the phenolic compound of example 1 of the present invention is applied to improve the humidity resistance of tetravalent manganese-doped potassium hexafluorosilicate, the humidity resistance can be improved. The state diagrams of the phosphors obtained in the embodiments 2 to 17 after being soaked in water for 24 hours under the irradiation of natural light/365 nm ultraviolet lamps are basically consistent with those of the phosphor obtained in the embodiment 1, which shows that the phenolic compounds can improve the humidity resistance of the tetravalent manganese fluoride red phosphor.
In each case 7 parts of 100mg of KSF and KSF-HQ as described in example 1 were prepared. 1ml of water was added to each of the control groups except for the control group which did not contact water, and the water was poured out at 1h,6h,24h,72h,168h, and 336h and then dried. Thus obtaining the KSF and KSF-HQ which are soaked in water for 0h,1h,6h,24h,72h,168h and 336h. Photoluminescence excitation/emission (PLE/PL) spectral curves of each sample at room temperature were measured using a fluorescence spectrophotometer (Edinburgh FSL 920) using a 450W xenon lamp as the excitation source.
FIG. 4 is a graph showing the luminescence intensity of the modified tetravalent manganese-doped potassium hexafluorosilicate (KSF-HQ) prepared in example 1 after different soaking times than that of the unmodified tetravalent manganese-doped potassium hexafluorosilicate (KSF). As can be seen from the figure, the modified KSF (KSF-HQ) has long-term stability in a water-rich environment, while the unmodified KSF has serious loss of luminescence property, which indicates that the phenolic compound described in example 1 does not reduce the luminescence property when being used for improving the humidity resistance of the tetravalent manganese fluoride red fluorescent powder. The luminous intensity graphs of the phosphors of the embodiments 2-17 after different soaking times are substantially the same as the luminous intensity graphs of the materials obtained in the embodiment 1 after different soaking times, which shows that the luminous performance of the red phosphor of tetravalent manganese fluoride can not be reduced when the phenolic compound is used for improving the humidity resistance of the red phosphor of tetravalent manganese fluoride.
Five groups of tetravalent manganese-doped potassium hexafluorosilicate (KSF) were prepared, each loaded with 5% by weight of each of bisphenol fluorene, m-triphenylphenol, p-diphenol, 1,5-dihydroxynaphthalene, and bisphenol A five phenols by chemisorption, and 10mg of each was put into a centrifuge tube, and 1ml of water was added thereto and observed. After 7 days, as shown in the following figure. The phenol loaded from left to right is bisphenol fluorene, phloroglucinol, hydroquinone, 1,5-hydroxynaphthalene and bisphenol A in turn, and no modification control is provided.
FIG. 5 is a graph of 460nm excited states of different phenol modified tetravalent manganese doped hexafluoro-silicon potassium and unmodified tetravalent manganese doped hexafluoro-silicon potassium after water immersion for 7 days. In the figure, the fluorescent powder in the left test tube 1 is tetravalent manganese doped potassium hexafluorosilicate modified by bisphenol fluorene, and the fluorescent powder in the left test tube 4 is tetravalent manganese doped potassium hexafluorosilicate modified by 1,5-dihydroxy naphthalene. As can be seen from the figure, the loss of the luminescence property of the bisphenol fluorene modified tetravalent manganese doped hexafluoro-silicon potassium and the 5-dihydroxy naphthalene modified tetravalent manganese doped hexafluoro-silicon potassium in water is quite serious, which shows that the phenol compounds described in comparative examples 2 and 3 can reduce the luminescence property of the tetravalent manganese fluoride red fluorescent powder when being used for improving the humidity resistance.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (9)
1. The application of the phenolic compound in improving the humidity resistance of the tetravalent manganese fluoride red fluorescent powder is characterized in that the phenolic compound is selected from one or more of hydroquinone, phloroglucinol and bisphenol A; the mass ratio of the tetravalent manganese fluoride red fluorescent powder to the phenolic compound is 1000: (5 to 50); the tetravalent manganese fluoride red fluorescent powder is tetravalent manganese-doped hexafluoro-silicon-potassium.
2. The use of claim 1, wherein the phenolic compound improves the moisture resistance of the tetravalent manganese fluoride red phosphor by:
dissolving a phenolic compound in an organic solvent, adding tetravalent manganese fluoride red fluorescent powder, and performing ultrasonic drying.
3. The use according to claim 1, wherein the method for improving the moisture resistance of the tetravalent manganese fluoride red phosphor by the phenolic compound comprises the steps of:
grinding the phenolic compound into powder with the particle size less than 5 mu m, adding tetravalent manganese fluoride red fluorescent powder, and uniformly mixing.
4. The use according to claim 1, wherein the mass ratio of the tetravalent manganese fluoride red phosphor to the phenolic compound is 1000: (5 to 25).
5. The use of claim 1, wherein the mass ratio of the tetravalent manganese fluoride red phosphor to the phenolic compound is 1000: (5 to 10).
6. The use according to claim 2, wherein the organic solvent is selected from one or more of ethyl ether, ethyl acetate and ethanol.
7. The use according to claim 2, wherein the tetravalent manganese fluoride red phosphor is added at 200 to 800mg per ml of organic solvent.
8. The use according to claim 7, wherein 200 to 500mg tetravalent manganese fluoride red phosphor is added per ml organic solvent.
9. The use according to claim 2, wherein the drying temperature is from 40 to 80 ℃.
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| CN107236543A (en) * | 2017-06-15 | 2017-10-10 | 华南理工大学 | One kind improves Mn4+The method of doped fluoride red fluorescence powder material moisture resistance properties |
| CN112251219A (en) * | 2020-10-29 | 2021-01-22 | 桂林理工大学 | Moisture-proof fluoride red fluorescent powder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107236543A (en) * | 2017-06-15 | 2017-10-10 | 华南理工大学 | One kind improves Mn4+The method of doped fluoride red fluorescence powder material moisture resistance properties |
| CN112251219A (en) * | 2020-10-29 | 2021-01-22 | 桂林理工大学 | Moisture-proof fluoride red fluorescent powder and preparation method thereof |
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| A new reductive DL-mandelic acid loading approach for moisture-stable Mn4+ doped fluorides;Lin Huang et al.;《Chem. Commun.》;20180828;第54卷;第11823-11976页 * |
| Improved Moisture-Resistant and Luminescence Properties of a Red Phosphor Based on Dodec-fluoride K3RbGe2F12:Mn4+ through Surface Modification;Yajun Jia et al.;《Inorg. Chem》;20201111;第60卷;第231-238页 * |
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