CN106118651B - A kind of preparation method of specular removal luminescent material - Google Patents
A kind of preparation method of specular removal luminescent material Download PDFInfo
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- CN106118651B CN106118651B CN201610467779.7A CN201610467779A CN106118651B CN 106118651 B CN106118651 B CN 106118651B CN 201610467779 A CN201610467779 A CN 201610467779A CN 106118651 B CN106118651 B CN 106118651B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title claims abstract description 16
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910020491 K2TiF6 Inorganic materials 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000011572 manganese Substances 0.000 abstract description 27
- 239000000843 powder Substances 0.000 abstract description 22
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 21
- 229910052748 manganese Inorganic materials 0.000 abstract description 21
- 239000011159 matrix material Substances 0.000 abstract description 10
- 239000003795 chemical substances by application Substances 0.000 abstract description 9
- 238000000295 emission spectrum Methods 0.000 abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 16
- 238000006467 substitution reaction Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 229910004820 CaTiF6 Inorganic materials 0.000 description 4
- 229910001634 calcium fluoride Inorganic materials 0.000 description 4
- 230000005284 excitation Effects 0.000 description 4
- 229910000590 K2MnF6 Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 2
- 229910020440 K2SiF6 Inorganic materials 0.000 description 1
- 229910021570 Manganese(II) fluoride Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- CTNMMTCXUUFYAP-UHFFFAOYSA-L difluoromanganese Chemical compound F[Mn]F CTNMMTCXUUFYAP-UHFFFAOYSA-L 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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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
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/674—Halogenides
- C09K11/675—Halogenides with alkali or alkaline earth metals
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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
- C09K11/615—Halogenides
- C09K11/616—Halogenides with alkali or alkaline earth metals
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The present invention relates to a kind of preparation method of specular removal luminescent material.It is with MeXTiF6For matrix, KMnO4For raw material, HF is solvent, and reacted under conditions of agent and reducing agent are provided added with part；Wherein, Me can be K, Na, Li plasma or be Ca, Mg plasma, and X phases should be 2~1.This preparation method has the advantages that quick, easy, cost is cheap, and the manganese base fluorescent powder that emission spectrum is red broad peak has been made in it under normal temperature and pressure conditionses.
Description
The present invention is Application No. 201510103741.7, the division Shen of the patent of invention on the applying date 2015 year 03 month 10
Please.
Technical field
The present invention relates to luminescent material technical field.
Background technology
Existing yellow fluorescent powder, lack red light portion in its emission spectrum, it is difficult to prepare high-color rendering, warm colour temperature it is white
Light LED lamp bead, it is impossible to meet the modern lighting requirement of high quality.
New non-rare earth luminous manganese base fluorescent powder, such as：K2TiF6:Mn4+、K2SiF6:Mn4+、K2GeF6:Mn4+、Cs2GeF6:
Mn4+、Cs2SnF6:Mn4+Deng fluorescent material, have the advantages that quantum efficiency is high, simple without self-absorption, preparation method, is ground extensively
Study carefully.However, the preparation method of existing manganese base fluorescent powder exist two it is obvious the problem of：First, it is necessary to synthesize in preparation process
Presoma K2MnF6, and K2MnF6Preparation process it is more complicated；Second, the emission spectrum of its product is red spike, to improving
The display of white light LEDs is unfavorable.
The content of the invention
It is an object of the invention to provide a kind of preparation method of specular removal luminescent material.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of specular removal luminescent material, is specifically followed the steps below：
（1）Under normal temperature and pressure conditionses, by KMnO4, part provide agent first add in HF solution, be stirring evenly and then adding into also
Former agent is reacted, and after question response, then through filtering, is cleaned, is dried so that presoma is made with methanol, ethanol or acetone
K2MnF5·H2O；The step（1）In, the dosage of each reaction mass is KMnO according to mol ratio4：Part provides agent：Reducing agent：HF
=1：0.1~2：0.1~4：1~400 is configured；
（2）By presoma K2MnF5·H2O、MeXTiF6、KMnO4, part agent is provided and added in HF solution, stir anti-
1~40 h is answered, is finally cleaned, dried with methanol, ethanol or acetone through filtering again；The step（2）In, the use of each reaction mass
Amount is K according to mol ratio2MnF5·H2O：MeXTiF6：KMnO4：Part provides agent： HF：=1：0.1~10000：0.1~5：0.1
~5:1~1500 is configured.
Obtain after testing：Using manganese base fluorescent powder made from above-mentioned preparation method, consisting of MeXTiF6:Mn4+, wherein,
Matrix is MeXTiF6, Mn elements substitution matrix MeXTiF6The content ratio of middle Ti elements is 0 at.% ＜ Mn at.% ＜ 20.0
at.%；And the excitation peak of the manganese base fluorescent powder is the nm of 460 nm ± 10nm and 365 nm ± 10, can with LED blue chips and
The luminous matching of mercury vapour；Its emission spectrum broadband emission between 580~660 nm：There is the emission peak of five intersections, be respectively
The nm of 590 nm ± 2, the nm of 604 nm ± 2, the nm of 616 nm ± 2, the nm of 635 nm ± 2 and the nm of 650 nm ± 2,
Wherein highest peak is the nm of 635 nm ± 2, and a width of nm of 10 nm ± 2 of half-peak of highest peak.Therefore, it can be assumed that product
For a kind of brand-new manganese base fluorescent powder.
The invention has the advantages that：
The present invention discloses a kind of preparation method of specular removal manganese base fluorescent powder, and the preparation method has quick, easy, cost
The advantages that cheap, the manganese base fluorescent powder that emission spectrum is red broad peak has been made in it under normal temperature and pressure conditionses；Products therefrom
Outstanding advantages of with broadband emission, specular removal, high colour developing, beneficial to the display for improving white light LEDs, it can be widely applied to Gao Pin
Matter lighting engineering, such as：High colour developing, the coating of warm colour temperature white-light LED encapsulation, fluorescent tube etc..
Brief description of the drawings
Fig. 1 is the XRD spectrums using the product obtained by the preparation method of manganese base fluorescent powder described in the embodiment of the present invention 1
Figure.
Fig. 2 is the EDS spectrums using the product obtained by the preparation method of manganese base fluorescent powder described in the embodiment of the present invention 1
Figure.
Fig. 3 is the exciting light using the product obtained by the preparation method of manganese base fluorescent powder described in the embodiment of the present invention 1
Spectrogram.
Fig. 4 is the transmitting light using the product obtained by the preparation method of manganese base fluorescent powder described in the embodiment of the present invention 1
Spectrogram.
Fig. 5 is the EDS spectrums using the product obtained by the preparation method of manganese base fluorescent powder described in the embodiment of the present invention 2
Figure.
Fig. 6 is the exciting light using the product obtained by the preparation method of manganese base fluorescent powder described in the embodiment of the present invention 2
Spectrogram.
Fig. 7 is the transmitting light using the product obtained by the preparation method of manganese base fluorescent powder described in the embodiment of the present invention 2
Spectrogram.
Embodiment
The present invention is specifically described below by embodiment, it is necessary to it is pointed out here that, following examples are only used
It is further detailed in the present invention, it is impossible to be interpreted as limiting the scope of the invention, the field is skilled in technique
Personnel can make some nonessential modifications and adaptations according to foregoing invention content to the present invention.
Embodiment 1
A kind of preparation method of specular removal manganese base fluorescent powder, it is specifically what is followed the steps below：
（1）Under normal temperature and pressure conditionses, by KMnO4, KF first add in HF solution, be stirring evenly and then adding into H2O2Carry out anti-
Should, after question response, then through filtering, cleaned, dried so that presoma K is made with methanol2MnF5·H2O；The step（1）In, respectively
The dosage of material is KMnO according to mol ratio4：KF：H2O2：HF =1：2：4：200 are configured；
（2）By presoma K2MnF5·H2O、K2TiF6、KMnO4, KF add HF solution in, stir reaction 40 h, most
Cleaned, dried with methanol through filtering again afterwards；The step（2）In, the dosage of each material is K according to mol ratio2MnF5·
H2O：K2TiF6：KMnO4：KF：HF=1：20：5：5:500 are configured.
Its in this example prepares the principle reacted：
KMnO4 + KF + 4HF + 2H2O2 → K2MnF5·H2O + 3H2O + 2O2 (1)
2K2MnF5·H2O→ K2MnF6 + MnF2 +2KF + H2O (2)
Wherein, KMnO4While promoting the progress of reaction (2), and react (2) progress, the Mn of generation4+With matrix
K2TiF6Also reacted so that Mn4+It is micro to instead of K2TiF6In Ti4+；React (2) and micro Mn4+Substitution reaction it is same
Shi Fasheng, mutually promote, finally realize in K2TiF6Middle introducing Mn4+And K is made2TiF6:Mn4+。
Understood with reference to the testing result shown in accompanying drawing 1,2,3 and 4：Using the manganese base fluorescence obtained by the preparation method
Powder, the agent structure of its crystal is matrix K2TiF6, Mn elements substitution matrix K2TiF6The content ratio of middle Ti elements is 5.75
At.%, its excitation peak are 463.4 nm and 363 nm, emission spectrum broadband emission between 580~660 nm：There are five intersections
Emission peak, respectively 590.0 nm, 603.6 nm, 616.2 nm, 634.6 nm and 650.4 nm, wherein highest peak is
634.6 nm, and a width of 10 nm of half-peak of highest peak.
Embodiment 2
A kind of preparation method of specular removal manganese base fluorescent powder, it is specifically what is followed the steps below：
（1）Under normal temperature and pressure conditionses, by KMnO4, KF first add in HF solution, be stirring evenly and then adding into H2O2Carry out anti-
Should, after question response, then through filtering, cleaned, dried so that presoma K is made with ethanol2MnF5·H2O；The step（1）In, respectively
The dosage of material is KMnO according to mol ratio4：KF：H2O2：HF =1：0.2：2：100 are configured；
（2）By presoma K2MnF5·H2O、K2TiF6、KMnO4, KF add HF solution in, stir reaction 10 h, most
Cleaned, dried with ethanol through filtering again afterwards；The step（2）In, the dosage of each material is K according to mol ratio2MnF5·
H2O：K2TiF6：KMnO4：KF：HF=1：0.1：0.5：0.5:100 are configured.
Understood with reference to the testing result shown in accompanying drawing 5,6 and 7：Using the manganese base fluorescent powder obtained by the preparation method,
The agent structure of its crystal is matrix K2TiF6, Mn elements substitution matrix K2TiF6The content ratio of middle Ti elements is 4.80
At.%, its excitation peak are 462.8 nm and 363 nm, can light and match with LED blue chips and mercury vapour, its emission spectrum exists
Broadband emission between 580~660 nm：Have five intersection emission peaks, respectively 590.2 nm, 603.2 nm, 616.2 nm,
634.8 nm and 650.4 nm, wherein highest peak are 634.8 nm, and a width of 10 nm of half-peak of highest peak.
Embodiment 3
A kind of preparation method of specular removal manganese base fluorescent powder, it is specifically what is followed the steps below：
（1）Under normal temperature and pressure conditionses, by KMnO4、CaF2First add in HF solution, be stirring evenly and then adding into ethanol progress
React, after question response, then through filtering, cleaned, dried so that presoma CaMnF is made with methanol5·H2O；The step（1）In,
The dosage of each material is KMnO according to mol ratio4：CaF2：Ethanol：HF =1：5：4：400 are configured；
（2）By presoma CaMnF5·H2O、CaTiF6、KMnO4、CaF2Add in HF solution, stir 10 h of reaction,
Finally cleaned again through filtering with methanol, prepared by drying；The step（2）In, the dosage of each material is according to mol ratio
CaMnF5·H2O：CaTiF6：KMnO4：CaF2：HF=1：100：5：5:1000 are configured.
After testing：Using the manganese base fluorescent powder obtained by the preparation method, the agent structure of its crystal is matrix CaTiF6,
Mn elements substitution matrix CaTiF6The content ratio of middle Ti elements is 8.50 at.%, and its excitation peak is 463.3 nm and 363.0
Nm, it can light and match with LED blue chips and mercury vapour, its emission spectrum broadband emission between 580~660 nm：There are five
The emission peak of intersection, respectively 590.5 nm, 603.3 nm, 616.5 nm, 634.0 nm and 650.4 nm, wherein highest peak are
634.0 nm, and a width of 10 nm of half-peak of highest peak.
Claims (1)
1. a kind of preparation method of specular removal luminescent material, it is specifically what is followed the steps below：
（1）Under normal temperature and pressure conditionses, by KMnO4, KF first add in HF solution, be stirring evenly and then adding into H2O2Reacted, treated
After completion of the reaction, then through filtering, cleaned, dried so that presoma K is made with ethanol2MnF5·H2O；The step（1）In, each material
Dosage according to mol ratio be KMnO4：KF：H2O2：HF =1：0.2：2：100 are configured；
（2）By presoma K2MnF5·H2O、K2TiF6、KMnO4, KF add HF solution in, stir reaction 10 h, finally again
Through filtering, cleaned, dried with ethanol；The step（2）In, the dosage of each material is K according to mol ratio2MnF5·H2O：
K2TiF6：KMnO4：KF：HF=1：0.1：0.5：0.5:100 are configured.
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| CN201510103741.7A CN104650876B (en) | 2015-03-10 | 2015-03-10 | A kind of preparation method of manganio fluorescent material |
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| CN105505384B (en) * | 2015-12-03 | 2017-12-19 | 河北利福光电技术有限公司 | A kind of narrow band red light fluorescent powder and preparation method thereof |
| CN110648859B (en) * | 2018-06-27 | 2021-04-16 | 南京理工大学 | TiO2Coating delta-MnO2Nano-sheet array composite material and preparation method thereof |
| CN110257065B (en) * | 2019-06-28 | 2022-05-17 | 重庆文理学院 | Red fluorescent powder with waterproof performance and preparation method thereof |
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| CN102732249A (en) * | 2011-04-08 | 2012-10-17 | 信越化学工业株式会社 | Preparation of complex fluoride and complex fluoride phosphor |
| CN103980896A (en) * | 2014-04-29 | 2014-08-13 | 中国科学院福建物质结构研究所 | Preparation method of fluoride fluorescent powder material |
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| JP5783302B2 (en) * | 2013-07-03 | 2015-09-24 | 日亜化学工業株式会社 | Fluoride phosphor, light emitting device using the same, and method for producing phosphor |
| JP5890810B2 (en) * | 2013-08-29 | 2016-03-22 | 株式会社東芝 | Switch circuit |
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| CN102732249A (en) * | 2011-04-08 | 2012-10-17 | 信越化学工业株式会社 | Preparation of complex fluoride and complex fluoride phosphor |
| CN103980896A (en) * | 2014-04-29 | 2014-08-13 | 中国科学院福建物质结构研究所 | Preparation method of fluoride fluorescent powder material |
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| CN106118651A (en) | 2016-11-16 |
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