CN106118651A - 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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- CN106118651A CN106118651A CN201610467779.7A CN201610467779A CN106118651A CN 106118651 A CN106118651 A CN 106118651A CN 201610467779 A CN201610467779 A CN 201610467779A CN 106118651 A CN106118651 A CN 106118651A
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- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910020491 K2TiF6 Inorganic materials 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000010926 purge Methods 0.000 claims description 4
- 239000000758 substrate Substances 0.000 abstract description 10
- 239000003795 chemical substances by application Substances 0.000 abstract description 8
- 238000000295 emission spectrum Methods 0.000 abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 abstract description 3
- 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 18
- 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
- 238000004020 luminiscence type Methods 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
- 238000000034 method Methods 0.000 description 2
- 239000000843 powder Substances 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
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process 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
- 238000005538 encapsulation Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 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
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction 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
- C09K11/61—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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- 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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- 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 the preparation method of a kind of specular removal luminescent material.It is with MeXTiF6For substrate, KMnO4For raw material, HF is solvent, and carries out reacting being added with under conditions of part provides agent and reducing agent；Wherein, Me can be K, Na, Li plasma or be Ca, Mg plasma, and X phase should be 2～1.This preparation method has the advantages such as quick, easy, with low cost, and it has i.e. prepared the manganio fluorescent material that emission spectrum is red broad peak under normal temperature and pressure conditions.
Description
The present invention is Application No. 201510103741.7, the division Shen of the patent of invention of on 03 10th, 2015 applying date
Please.
Technical field
The present invention relates to luminescent material technical field.
Background technology
Existing yellow fluorescent powder, lacks red light portion in its emission spectrum, it is difficult to prepare high-color rendering, warm colour temperature white
Light LED lamp bead, it is impossible to meet high-quality modern lighting requirement.
Novel non-rare earth luminous manganio fluorescent material, such as: K2TiF6:Mn4+、K2SiF6:Mn4+、K2GeF6:Mn4+、Cs2GeF6:
Mn4+、Cs2SnF6:Mn4+In fluorescent material, have quantum efficiency high, without self-absorption, the preparation method advantage such as simply, extensively ground
Study carefully.But, there are two obvious problems in the preparation method of existing manganio fluorescent material: one is in preparation process, needs synthesis
Presoma K2MnF6, and K2MnF6Preparation process more complicated；Two is that the emission spectrum of its product is red spike, to raising
The display of white light LEDs is unfavorable.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of specular removal luminescent material.
It is an object of the invention to be achieved through the following technical solutions:
The preparation method of a kind of specular removal luminescent material, specifically follows the steps below:
(1) under normal temperature and pressure conditions, by KMnO4, part provide agent be initially charged in HF solution, be stirring evenly and then adding into reducing agent
React, after question response, then through sucking filtration, clean with methanol, ethanol or acetone, be dried with prepared presoma K2MnF5·
H2O；In this step (1), the consumption of each reaction mass is KMnO according to mol ratio4: part offer agent: reducing agent: HF=1:0.1
～2:0.1～4:1～400 configures；
(2) by presoma K2MnF5·H2O、MeXTiF6、KMnO4, part provide agent to add in HF solution, stir reaction 1～
40 h, the most again through sucking filtration, clean with methanol, ethanol or acetone, are dried；In this step (2), the consumption of each reaction mass according to
Mol ratio is K2MnF5·H2O:MeXTiF6: KMnO4: part provides agent: HF:=1:0.1～10000:0.1～5:0.1～5:1
～1500 configure.
Obtain after testing: use the manganio fluorescent material that above-mentioned preparation method prepares, consisting of MeXTiF6:Mn4+, wherein,
Substrate is MeXTiF6, Mn element replaces substrate MeXTiF6The content ratio of middle Ti element is 0 at.% ＜ Mn at.% ＜ 20.0
at.%；And the excitation peak of this manganio fluorescent material is 460 nm ± 10nm and 365 nm ± 10 nm, can with LED blue chip and
Mercury vapour luminescence is mated；Its emission spectrum is broadband emission between 580～660 nm: have five emission peaks intersected, and is respectively
590 nm ± 2 nm, 604 nm ± 2 nm, 616 nm ± 2 nm, 635 nm ± 2 nm and 650 nm ± 2 nm,
Wherein highest peak is 635 nm ± 2 nm, and a width of 10 nm ± 2 nm of half-peak of highest peak.Therefore, it can assert product
For a kind of brand-new manganio fluorescent material.
The method have the advantages that
The present invention discloses the preparation method of a kind of specular removal manganio fluorescent material, and this preparation method has quick, easy, with low cost
Etc. advantage, it has i.e. prepared the manganio fluorescent material that emission spectrum is red broad peak under normal temperature and pressure conditions；Products therefrom has
The outstanding advantages such as broadband emission, specular removal, high colour developing, are beneficial to improve the display of white light LEDs, can be widely applied to high-quality and shine
Bright technology, such as: high colour developing, warm colour temperature white-light LED encapsulation, fluorescent tube coating etc..
Accompanying drawing explanation
Fig. 1 is the XRD spectrum using the product obtained by preparation method of manganio fluorescent material described in the embodiment of the present invention 1
Figure.
Fig. 2 is the EDS spectrum using the product obtained by preparation method of manganio fluorescent material described in the embodiment of the present invention 1
Figure.
Fig. 3 is to use the exciting light of the product obtained by preparation method of manganio fluorescent material described in the embodiment of the present invention 1
Spectrogram.
Fig. 4 is to use the transmitting light of the product obtained by preparation method of manganio fluorescent material described in the embodiment of the present invention 1
Spectrogram.
Fig. 5 is the EDS spectrum using the product obtained by preparation method of manganio fluorescent material described in the embodiment of the present invention 2
Figure.
Fig. 6 is to use the exciting light of the product obtained by preparation method of manganio fluorescent material described in the embodiment of the present invention 2
Spectrogram.
Fig. 7 is to use the transmitting light of the product obtained by preparation method of manganio fluorescent material described in the embodiment of the present invention 2
Spectrogram.
Detailed description of the invention
Below by embodiment, the present invention is specifically described, it is necessary to it is pointed out here that, following example are only used
In the present invention is further detailed, it is impossible to be interpreted as limiting the scope of the invention, being skilled in technique of this field
The present invention can be made some nonessential improvement and adjustment according to foregoing invention content by personnel.
Embodiment 1
A kind of preparation method of specular removal manganio fluorescent material, it specifically follows the steps below:
(1) under normal temperature and pressure conditions, by KMnO4, KF be initially charged in HF solution, be stirring evenly and then adding into H2O2React, treat
After completion of the reaction, then through sucking filtration, clean with methanol, be dried with prepared presoma K2MnF5·H2O；In this step (1), each material
Consumption be KMnO according to mol ratio4: KF:H2O2: HF=1:2:4:200 configures；
(2) by presoma K2MnF5·H2O、K2TiF6、KMnO4, KF add in HF solution, stir reaction 40 h, the most again
Through sucking filtration, clean with methanol, be dried；In this step (2), the consumption of each material is K according to mol ratio2MnF5·H2O:
K2TiF6: KMnO4: KF:HF=1:20:5:5:500 configures.
In this example, the principle of its preparation reaction is:
KMnO4 + KF + 4HF + 2H2O2 → K2MnF5·H2O + 3H2O + 2O2 (1)
2K2MnF5·H2O→ K2MnF6 + MnF2 +2KF + H2O (2)
Wherein, KMnO4Promote the carrying out of reaction (2), and while reaction (2) is carried out, the Mn of generation4+With substrate K2TiF6Also
React so that Mn4+Trace instead of K2TiF6In Ti4+；Reaction (2) and trace Mn4+Substitution reaction occur simultaneously, phase
Promote mutually, finally achieve at K2TiF6Middle introducing Mn4+And prepared K2TiF6:Mn4+。
Understand in conjunction with the testing result shown in accompanying drawing 1,2,3 and 4: use the manganio fluorescence obtained by this preparation method
Powder, the agent structure of its crystal is substrate K2TiF6, Mn element replaces substrate K2TiF6The content ratio of middle Ti element is 5.75
At.%, its excitation peak is 463.4 nm and 363 nm, and emission spectrum is broadband emission between 580～660 nm: have 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 manganio fluorescent material, it specifically follows the steps below:
(1) under normal temperature and pressure conditions, by KMnO4, KF be initially charged in HF solution, be stirring evenly and then adding into H2O2React, treat
After completion of the reaction, then through sucking filtration, with ethanol purge, it is dried with prepared presoma K2MnF5·H2O；In this step (1), each material
Consumption be KMnO according to mol ratio4: KF:H2O2: HF=1:0.2:2:100 configures；
(2) by presoma K2MnF5·H2O、K2TiF6、KMnO4, KF add in HF solution, stir reaction 10 h, the most again
Through sucking filtration, with ethanol purge, it is dried；In this step (2), the consumption of each material is K according to mol ratio2MnF5·H2O:
K2TiF6: KMnO4: KF:HF=1:0.1:0.5:0.5:100 configures.
Understand in conjunction with the testing result shown in accompanying drawing 5,6 and 7: use the manganio fluorescent material obtained by this preparation method,
The agent structure of its crystal is substrate K2TiF6, Mn element replaces substrate K2TiF6The content ratio of middle Ti element is 4.80
At.%, its excitation peak is 462.8 nm and 363 nm, can mate with LED blue chip and mercury vapour luminescence, and its emission spectrum exists
Broadband emission between 580～660 nm: have five emission peaks intersected, respectively 590.2 nm, 603.2 nm, 616.2 nm,
634.8 nm and 650.4 nm, wherein highest peak is 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 manganio fluorescent material, it specifically follows the steps below:
(1) under normal temperature and pressure conditions, by KMnO4、CaF2It is initially charged in HF solution, is stirring evenly and then adding into ethanol and carries out instead
Should, after question response, then through sucking filtration, clean with methanol, be dried with prepared presoma CaMnF5·H2O；In this step (1), respectively
The consumption of material is KMnO according to mol ratio4: CaF2: ethanol: HF=1:5:4:400 configures；
(2) by presoma CaMnF5·H2O、CaTiF6、KMnO4、CaF2Adding in HF solution, stir reaction 10 h, finally
Again through sucking filtration, clean with methanol, dry and prepared；In this step (2), the consumption of each material is CaMnF according to mol ratio5·
H2O:CaTiF6: KMnO4: CaF2: HF=1:100:5:5:1000 configures.
After testing: use the manganio fluorescent material obtained by this preparation method, the agent structure of its crystal is substrate CaTiF6,
Mn element replaces substrate CaTiF6The content ratio of middle Ti element is 8.50 at.%, and its excitation peak is 463.3 nm and 363.0
Nm, can mate with LED blue chip and mercury vapour luminescence, and its emission spectrum is broadband emission between 580～660 nm: have five
The emission peak intersected, respectively 590.5 nm, 603.3 nm, 616.5 nm, 634.0 nm and 650.4 nm, wherein highest peak is
634.0 nm, and a width of 10 nm of half-peak of highest peak.
Claims (1)
1. a preparation method for specular removal luminescent material, it specifically follows the steps below:
(1) under normal temperature and pressure conditions, by KMnO4, KF be initially charged in HF solution, be stirring evenly and then adding into H2O2React, treat
After completion of the reaction, then through sucking filtration, with ethanol purge, it is dried with prepared presoma K2MnF5·H2O；In this step (1), each material
Consumption be KMnO according to mol ratio4: KF:H2O2: HF=1:0.2:2:100 configures；
(2) by presoma K2MnF5·H2O、K2TiF6、KMnO4, KF add in HF solution, stir reaction about 10 h, finally
Again through sucking filtration, with ethanol purge, it is dried；In this step (2), the consumption of each material is K according to mol ratio2MnF5·H2O:
K2TiF6: KMnO4: KF:HF=1:0.1:0.5:0.5:100 configures.
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| CN201610467779.7A CN106118651B (en) | 2015-03-10 | 2015-03-10 | A kind of preparation method of specular removal luminescent material |
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| CN201510103741.7A CN104650876B (en) | 2015-03-10 | 2015-03-10 | A kind of preparation method of manganio fluorescent material |
| CN201610467779.7A CN106118651B (en) | 2015-03-10 | 2015-03-10 | A kind of preparation method of specular removal luminescent material |
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| CN201610467808.XA Expired - Fee Related CN105950138B (en) | 2015-03-10 | 2015-03-10 | A kind of preparation method of the fluorescent material with red broad peak emission spectrum |
| CN201610468090.6A Active CN106085428B (en) | 2015-03-10 | 2015-03-10 | A kind of fluorescent material suitable for LED illumination |
| CN201510103741.7A Expired - Fee Related CN104650876B (en) | 2015-03-10 | 2015-03-10 | A kind of preparation method of manganio fluorescent material |
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| CN201610468090.6A Active CN106085428B (en) | 2015-03-10 | 2015-03-10 | A kind of fluorescent material suitable for LED illumination |
| CN201510103741.7A Expired - Fee Related 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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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| US20150061748A1 (en) * | 2013-08-29 | 2015-03-05 | Kabushiki Kaisha Toshiba | Switch circuit |
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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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US20150061748A1 (en) * | 2013-08-29 | 2015-03-05 | Kabushiki Kaisha Toshiba | Switch circuit |
| 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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| CN104650876A (en) | 2015-05-27 |
| CN106085428B (en) | 2018-02-23 |
| CN104650876B (en) | 2016-07-13 |
| CN106085428A (en) | 2016-11-09 |
| CN105950138B (en) | 2018-01-30 |
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