CN106544010A - A kind of preparation method of MOF bases white emitting fluorescent powder - Google Patents
A kind of preparation method of MOF bases white emitting fluorescent powder Download PDFInfo
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- CN106544010A CN106544010A CN201610945248.4A CN201610945248A CN106544010A CN 106544010 A CN106544010 A CN 106544010A CN 201610945248 A CN201610945248 A CN 201610945248A CN 106544010 A CN106544010 A CN 106544010A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- C—CHEMISTRY; METALLURGY
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
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Abstract
The invention provides a kind of MOF bases white emitting fluorescent powder, including one utilizes ZrCl4The step of synthesizing ZrBDC metal-organic framework materials with p-phthalic acid；By Eu3+And Tb3+It is dissolved in solvent dimethylformamide, obtains mixed liquor；ZrBDC substrate is placed in prepared mixed solution, flow back at 60 80 DEG C 8 ~ 10h, sucking filtration, dry acquisition MOF base white emitting fluorescent powders.Method of the present invention using substep modification, by MOF substrate and luminophore organic coupling, realizes white light emission.Preparation method host material structure-controllable, central ion concentration is adjustable, easily realizes spectrum cutting.Under 280nm ultraviolet excitations, the chromaticity coordinates of fluorescent material exists the MOF fluorescent materials for being obtained（0.3366,0.3451）, belong to white light emission.In addition, at 450 DEG C, stable luminescent property.
Description
Technical field
The invention belongs to materialogy field, is related to a kind of rare earth luminescent material, it is specifically a kind of that there is high heat stability
Property, be readily synthesized and MOF base white emitting fluorescent powders that luminous intensity is high preparation method.
Background technology
White light emitting diodes（WLEDs）Have that energy consumption is low, size is little because of which, be widely used efficiency high, life-span length
In green illumination, display and other electrooptical devices.Producing white light LEDs in the market mainly has two schemes, and scheme one is
Utilize " Blue-Ray technology " to coordinate with yellow fluorescent powder and obtain white light emission fluorescent material, but as the disappearance of red spectrum causes it to deposit
The problem poor in color reducibility, colour temperature is high, color rendering index is low；Scheme two is by adjusting multiple different single luminous fluorescents
Obtaining white light, although this method supplements red light region spectrum to powder, overcomes the problem of the presence of scheme one, but multiphase fluorescence
Powder is used in mixed way the difficulty that increased coating processes, while bringing, luminous efficiency is reduced, service life is low, color stability
Difference, a series of problems, such as photoluminescent band is narrow.Metal-organic framework material（MOFs）It is to develop swift and violent one kind in recent ten years newly
Emerging porous material, it is the crystalline material formed by self assembly by inorganic metal center and organic ligand, due to MOF materials
With structure diversity and porous feature, thus separation and storage, the medicine of gas are widely used in as medium carrier
The fields such as thing transport, catalysis, luminescent material.The inorganic metal center contained in MOF materials, organic ligand, guest molecule, and
Electron transfer between metal center and organic ligand, the electron transfer between metal center and metal center, organic ligand with
Electron transfer between organic ligand allows it to become a kind of preferable ultraviolet LED excitation light-emitting material.Additionally, luminous face
Color can also be regulated and controled by the species of doping with rare-earth ions and concentration and guest species and excitation wavelength.These advantages make
MOF materials have great using value in white light emission.Rare earth usually has the laudatory title of " industrial vitamin ", China's Rare Earth Mine
Hide abundant, account for more than the 40% of world's gross reserves, and total class is complete, this provides sound assurance for the application of rare earth.Rare earth from
Son is widely applied in fields such as light, electricity, magnetic due to its special electron structure, is especially sending out Material Field, and design is simultaneously
The rare earth luminescent material that synthesis luminous intensity is high, practical value is good is always the target that researchers pursue.The 4f of rare earth ion
Electronic shell when receiving illumination and exciting, is affected smaller by Ligand Field, thus can be produced due to by outer-shell electron shielding action
The narrow and strong characteristic emission of life, luminance purity are higher.But due to the absorbance of rare earth ion it is low so that it must pass through part
Formation " sensitized fluorescence " effect sets up energy transmission could strengthen ionoluminescence.Therefore, rare earth metal-organic frame has due to which
The excellent photoluminescent property that has and become study hotspot.
A kind of rare earth metal organic frame fluorescent sensing material is disclosed in patent CN102617615B, the program is utilized
The sodium salt of thioglycolic acid stannum is with neodymium nitrate by the method synthesizing rare-earth metal framework material for crystallizing, sulfur in reaction is evaporated under reduced pressure
There is coordination polymerization with rare earth ion for glycolic stannum anion.The material is stable in the air, is difficult to be corroded, not with commonly
Acid, alkali and organic solvent reaction, but the reaction condition is more harsh, and its heat stability only has 300 DEG C, and due to this
Case is that rare earth ion directly occurs coordination polymerization with organic ligand, thus course of reaction Rare Earth Ion concentration can not regulate and control.
The content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of preparation side of MOF bases white emitting fluorescent powder
Method, the preparation method of described this MOF bases white emitting fluorescent powder will solve the hot steady of MOF fluorescent materials presence of the prior art
Qualitative difference, preparation condition are harsh, the technical problem that central ion concentration can not regulate and control.
The invention provides a kind of preparation method of MOF bases white emitting fluorescent powder, comprises the steps：
1) in molar ratio 1：（1~1.2）Ratio weigh ZrCl4And p-phthalic acid（H2BDC）, it is dissolved in dimethylformamide,
According to volume ratio of the dimethylformamide with acetic acid it is（10~12）：1 ratio adds acetic acid, is placed in one with politef
In reactor for liner bottle, reaction temperature is 160 ~ 180 DEG C, and the time is 20 ~ 24h, after being cooled to room temperature, sucking filtration, and use two
Methylformamide is washed, and obtains ZrBDC substrate after dry, grinding；
2) by Eu3+And Tb3+It is x in molar ratio:The ratio of 1-x is dissolved in solvent dimethylformamide, 0.4≤x≤0.45, control
Eu processed3+Concentration is 0.0001 ~ 0.0005mol/L, obtains dimethylformamide mixed liquor；
3) ZrBDC substrate is placed in into step 2）In in prepared mixed solution, step 2）Dimethylformamide mixed liquor with
The volume ratio of ZrBDC substrate is（8~10）：1, flow back at 60-80 DEG C 8 ~ 10h, sucking filtration, dry acquisition MOF base white fluorescences
Powder.
Further, Eu3+Selected from Eu (NO3)3·6H2O；Tb3+Selected from Tb (NO3)3·6H2O。
The present invention first adopts solvent-thermal method, synthesizes ZrBDC metal-organic framework materials（MOF）As host material；Make again
Standby Eu3+With Tb3+Dimethylformamide saline solution；Finally, using infusion process just gained ZrBDC substrate and Eu3+With Tb3+'s
Dimethylformamide saline solution mixed liquor flows back at 60-80 DEG C 8 ~ 10h, sucking filtration, is dried, and obtains MOF base white lights glimmering after grinding
Light powder.
Method of this patent using substep modification, MOF substrate and luminophore organic coupling are prepared using solvent-thermal method
Go out ZrBDC substrate, rare earth ion is injected in the duct of substrate by infusion method, white emitting fluorescent powder is obtained, white light is realized
Transmitting.In preparation process, host material structure-controllable, central ion concentration is adjustable, easily realizes spectrum cutting.Obtained
Under 280nm ultraviolet excitations, the chromaticity coordinates of fluorescent material exists MOF fluorescent materials（0.3366,0.3451）, belong to white light emission.
In addition, at 450 DEG C, stable luminescent property.The excitation wavelength of gained white emitting fluorescent powder of the invention is located at 250-330nm scopes,
Main excitation peak is located at 280nm, and under ultraviolet excitation, the peak-peak of emission spectrum is located at 545nm and 618nm, fluorescence respectively
The glow color of powder is white light, with up to 450 DEG C heat stability.
The present invention is compared with prior art, and its technological progress is significant.The fluorescent material of the present invention is suitable as ultraviolet sharp
The LED white emitting fluorescent powders sent out.Under ultraviolet excitation, the peak-peak of emission spectrum is located at 545nm and 618nm respectively, glimmering
The glow color of light powder is white, and luminous intensity is high.The fluorescent material of the present invention has high thermal stability, lights at 450 DEG C
It is stable.And in the preparation process of the present invention, Eu3+And Tb3+Ratio and concentration be easy to regulation and control, it is simple efficiently, preparation method letter
It is single, it is easy to practical application.
Description of the drawings
Fig. 1 is the Eu of the present invention3+ 0.4Tb3+ 0.6The emission spectrum of@ZrBDC.
Fig. 2 is this bright Eu3+ 0.4Tb3+ 0.6The chromaticity coordinate figure of@ZrBDC.
Specific embodiment
The present invention is expanded on further below by specific embodiment, but is not intended to limit the present invention.
Embodiment 1
A kind of MOF bases white emitting fluorescent powder, its preparation are comprised the following steps：
A. in molar ratio 1：1 ratio weighs 0.234gZrCl4With 0.168g p-phthalic acids（H2BDC）, it is dissolved in 10ml diformazans
Base Methanamide, is 10 according to the volume ratio of dimethylformamide and acetic acid：1 ratio Deca 1ml acetic acid, is placed in polytetrafluoroethyl-ne
Alkene is for, in the reactor of liner bottle, temperature is 160 DEG C, and the time is 20h；After being cooled to room temperature, sucking filtration, and use dimethylformamide
Washing three times, obtains ZrBDC substrate after drying and grinding；
B. by Eu (NO3)3·6H2O and Tb (NO3)3·6H2O is 0.4 in molar ratio:0.6 ratio is dissolved in 10ml dimethyl methyls
Amide, controls Eu3+Concentration is 0.0001mol/L, obtains dimethylformamide mixed liquor.
C. the volume ratio for pressing solution with powder is 8：1.25mlZrBDC substrate is placed in prepared in b mixing by 1 ratio
Close in liquid, flow back at 60 DEG C 10h, sucking filtration, dry acquisition MOF base white emitting fluorescent powders.
When excitation wavelength is 280nm, the fluorescence spectra of the fluorescent material is as shown in figure 1, the peak-peak of emission spectrum
It is located at 545nm and 618nm respectively, the glow color of fluorescent material is white light, chromaticity coordinates is（0.3366,0.3451）（Such as Fig. 2 institutes
Show）.
Embodiment 2
A kind of MOF bases white emitting fluorescent powder, its preparation are comprised the following steps：
A. in molar ratio 1：1.1 ratio weighs 0.234g ZrCl4With 0.185g p-phthalic acids（H2BDC）, it is dissolved in 10ml
Dimethylformamide, is 11 according to the volume ratio of dimethylformamide and acetic acid：1 ratio Deca 0.9ml acetic acid, is placed in poly-
Tetrafluoroethene is for, in the reactor of liner bottle, temperature is 170 DEG C, and the time is 22h；After being cooled to room temperature, sucking filtration, and use dimethyl
Methanamide is washed three times, and ZrBDC substrate is obtained after drying and grinding；
B. by Eu (NO3)3·6H2O and Tb (NO3)3·6H2O is 0.425 in molar ratio:0.575 ratio is dissolved in 10ml diformazans
Base Methanamide, controls Eu3+Concentration is 0.0003mol/L, obtains dimethylformamide mixed liquor；
C. the volume ratio for pressing solution with powder is 9：1.1mlZrBDC substrate is placed in mixed liquor prepared in b by 1 ratio
In, flow back at 70 DEG C 9h, sucking filtration, dry acquisition MOF base white emitting fluorescent powders.
When excitation wavelength is 280nm, the peak-peak of emission spectrum is located at 545nm and 618nm respectively, and fluorescent material is sent out
Light color is white, and its chromaticity coordinates is（0.3268,0.3370）.
Embodiment 3
A kind of MOF bases white emitting fluorescent powder, its preparation are comprised the following steps：
A. in molar ratio 1：1.2 ratio weighs 0.234g ZrCl4With 0.202g p-phthalic acids（H2BDC）, it is dissolved in 10ml
Dimethylformamide, is 12 according to the volume ratio of dimethylformamide and acetic acid：1 ratio Deca 0.8ml acetic acid, is placed in poly-
Tetrafluoroethene is for, in the reactor of liner bottle, temperature is 180 DEG C, and the time is 24h；After being cooled to room temperature, sucking filtration, and use dimethyl
Methanamide is washed three times, and ZrBDC substrate is obtained after drying and grinding；
B. by Eu (NO3)3·6H2O and Tb (NO3)3·6H2O is 0.45 in molar ratio:0.55 ratio is dissolved in 10ml dimethyl
Methanamide, controls Eu3+Concentration is 0.0005mol/L, obtains dimethylformamide mixed liquor；
C. the volume ratio for pressing solution with powder is 10：1 ratio is placed in 1mlZrBDC substrate in mixed liquor prepared in c,
Flow back at 80 DEG C 8h, sucking filtration, dry acquisition MOF base white emitting fluorescent powders.
When excitation wavelength is 280nm, the peak-peak of emission spectrum is located at 545nm and 618nm respectively, and fluorescent material is sent out
Light color is white light, and its chromaticity coordinates is（0.3345,0.3421）.
Claims (2)
1. a kind of preparation method of MOF bases white emitting fluorescent powder, it is characterised in that comprise the steps：
1）In molar ratio 1：（1~1.2）Ratio weigh ZrCl4And p-phthalic acid, it is dissolved in dimethylformamide, according to diformazan
Base Methanamide with the volume ratio of acetic acid is（10~12）：1 ratio adds acetic acid, is placed in one with politef as liner bottle
Reactor in, reaction temperature is 160 ~ 180 DEG C, and the time is 20 ~ 24h, after being cooled to room temperature, sucking filtration, and use dimethyl formyl
Amine is washed, and obtains ZrBDC substrate after dry, grinding；
2）By Eu3+And Tb3+It is x in molar ratio:The ratio of 1-x is dissolved in solvent dimethylformamide, 0.4≤x≤0.45, control
Eu3+Concentration is 0.0001 ~ 0.0005mol/L, obtains dimethylformamide mixed liquor；
3）ZrBDC substrate is placed in into step 2）In in prepared mixed solution, step 2）Dimethylformamide mixed liquor with
The volume ratio of ZrBDC substrate is（8~10）：1, flow back at 60-80 DEG C 8 ~ 10h, sucking filtration, dry acquisition MOF base white fluorescences
Powder.
2. the preparation method of a kind of MOF bases white emitting fluorescent powder according to claim 1, it is characterised in that including following step
Suddenly：Eu3+Preferably Eu (NO3)3·6H2O；Tb3+Selected from Tb (NO3)3·6H2O。
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107698775A (en) * | 2017-09-29 | 2018-02-16 | 成都理工大学 | More rare earth organic framework materials for white light emission and preparation method thereof |
| CN108164716A (en) * | 2018-02-13 | 2018-06-15 | 成都理工大学 | The method for preparing the organic MOFs materials of gadolinium matrix rare earth for white light emission |
| RU2686901C1 (en) * | 2017-03-31 | 2019-05-06 | Тойота Дзидося Кабусики Кайся | Organometallic structure and method of its production |
| CN109957113A (en) * | 2019-03-01 | 2019-07-02 | 南京工业大学 | A kind of Ce-MOF shines adjustable crystalline material and preparation method thereof and luminous regulation method |
| CN110305657A (en) * | 2019-06-17 | 2019-10-08 | 五邑大学 | A method of improving nitride red fluorescent powder luminescent properties with MOF material |
| CN110734761A (en) * | 2019-10-29 | 2020-01-31 | 南京邮电大学 | Preparation method and application of two-primary-color white light OLED material |
| RU2716125C1 (en) * | 2018-07-05 | 2020-03-05 | Тойота Дзидося Кабусики Кайся | Method of producing a coordinatively unsaturated metal-organic framework and a coordinatively unsaturated metal-organic framework |
| CN112625255A (en) * | 2019-11-28 | 2021-04-09 | 福建农林大学 | Synthetic method and application of proportional fluorescent probe for quantitatively detecting hypochlorite ions |
| CN114874243A (en) * | 2022-06-21 | 2022-08-09 | 江西省科学院应用化学研究所 | Double-rare-earth metal center white light fluorescent powder and preparation method and application thereof |
-
2016
- 2016-10-26 CN CN201610945248.4A patent/CN106544010A/en active Pending
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2686901C1 (en) * | 2017-03-31 | 2019-05-06 | Тойота Дзидося Кабусики Кайся | Organometallic structure and method of its production |
| US10702851B2 (en) | 2017-03-31 | 2020-07-07 | Toyota Jidosha Kabushiki Kaisha | Metal-organic framework and method of manufacturing the same |
| CN107698775A (en) * | 2017-09-29 | 2018-02-16 | 成都理工大学 | More rare earth organic framework materials for white light emission and preparation method thereof |
| CN107698775B (en) * | 2017-09-29 | 2020-07-14 | 成都理工大学 | Multi-rare earth-organic framework material for white light emission and preparation method thereof |
| CN108164716A (en) * | 2018-02-13 | 2018-06-15 | 成都理工大学 | The method for preparing the organic MOFs materials of gadolinium matrix rare earth for white light emission |
| RU2716125C1 (en) * | 2018-07-05 | 2020-03-05 | Тойота Дзидося Кабусики Кайся | Method of producing a coordinatively unsaturated metal-organic framework and a coordinatively unsaturated metal-organic framework |
| CN109957113A (en) * | 2019-03-01 | 2019-07-02 | 南京工业大学 | A kind of Ce-MOF shines adjustable crystalline material and preparation method thereof and luminous regulation method |
| CN110305657A (en) * | 2019-06-17 | 2019-10-08 | 五邑大学 | A method of improving nitride red fluorescent powder luminescent properties with MOF material |
| CN110734761A (en) * | 2019-10-29 | 2020-01-31 | 南京邮电大学 | Preparation method and application of two-primary-color white light OLED material |
| CN112625255A (en) * | 2019-11-28 | 2021-04-09 | 福建农林大学 | Synthetic method and application of proportional fluorescent probe for quantitatively detecting hypochlorite ions |
| CN112625255B (en) * | 2019-11-28 | 2022-02-01 | 福建农林大学 | Synthetic method and application of proportional fluorescent probe for quantitatively detecting hypochlorite ions |
| CN114874243A (en) * | 2022-06-21 | 2022-08-09 | 江西省科学院应用化学研究所 | Double-rare-earth metal center white light fluorescent powder and preparation method and application thereof |
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