CN108329909A - Macropore mayenite fluorescent material and preparation method thereof - Google Patents
Macropore mayenite fluorescent material and preparation method thereof Download PDFInfo
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- CN108329909A CN108329909A CN201810094516.5A CN201810094516A CN108329909A CN 108329909 A CN108329909 A CN 108329909A CN 201810094516 A CN201810094516 A CN 201810094516A CN 108329909 A CN108329909 A CN 108329909A
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- mayenite
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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
- C09K11/7743—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
- C09K11/7749—Aluminates
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Abstract
The invention discloses a kind of preparation methods of macropore mayenite fluorescent material, include the following steps：1), at room temperature, phase separation derivant is dissolved in the mixed solvent, after magnetic agitation, it adds the Aluminium chloride hexahydrate as presoma, CALCIUM CHLORIDE DIHYDRATE and nine chloride hydrate terbiums is added, drying control agent, chelating agent, after stirring evenly, gel accelerating agent ultrasound is added 50~70 seconds；2), the sol liquid obtained by step 1) is placed in closed container, in 50~70 DEG C of gels and is aged 24 ± 2h；3), gel after the ageing obtained by step 2) is placed in container, and in 50~70 DEG C of dry 3~4d；Then it is heat-treated 2~3h in 900~1300 DEG C, obtains macropore mayenite fluorescent material.The doped rare earth element mayenite fluorescent material that pore-size is controllable, porosity is higher, with coherent macroporous structure can be obtained using this method.
Description
Technical field
The invention belongs to the preparation fields of macropore mayenite fluorescent material, and in particular to one kind having co-continuous macroporous structure
Mayenite fluorescent material preparation method.
Background technology
In recent years, it the research of rare earth element and mixes the research of rare earth luminescent material and is obtained for development at full speed.But
Rare earth be there is a problem that expensive, therefore how effectively to be reduced material cost, and improve its luminous efficiency, is become research people
The focus that members are concerned about.Tb3+Green fluorescence can be emitted, luminous intensity is high, and quantum efficiency is high, and the sensibility of local area environment is high
The features such as, it is frequently used to the basic physics characteristic of research material.Therefore Tb3+As typical rear-earth-doped ion, each
All widely paid attention to and studied in field.Tb3+Excitation state5D4Energy level arrives7F5The transition spectral line of emission of energy level is in green light
Compose area, the green emitting phosphor Gd of Tb doping2O2S:Tb3+、Y2O2S:Tb3+、YAG:Tb3+、Y2SiO5:Tb3+Deng at present in many necks
Domain such as CRT, FED, lamp rare earth phosphor and scintillator etc. are widely used.But monochromaticjty is poor, thermal stability is not good enough
The problems such as still restrict the development of rare earth phosphor.Therefore find it is new take into account monochromaticjty, thermal stability, cost problem collection
There is major and immediate significance for illumination and field of color displays at multifunctional rare-earth doped substrate material.
Want to obtain rare earth luminescent material with high performance, the selection of matrix is even more important.Mayenite (Ca12Al14O33,
C12A7 just it is) a kind of broad-band gap oxide material that the thermal stability that more case substitutions occur is good, mayenite is CaO-Al2O3
There is a kind of functional material of great application prospect in binary system cubic crystal structure, each unit cell to be made of 118 atoms
Chemical formula [Ca24Al28O64]4+·2O2-, the positively charged structure that front portion is made of 12 crystallography cage structures, remaining
Two oxygen atoms occupy two in 12 Ca-Al-O cages, and Ca2+,Al3+Surrounding crystalline field is by O2-The modulation of group, symmetrically
Relatively low, the Tb of calcium ion and doping on low-symmetry case of property3+Radius is close therefore is easy to be replaced by it；C12A7, which has, to be received
The characteristics of rice positively charged cage cavity configuration, the abstinence for being easy to rare earth ion Uniform Doped and 4f electron transitions release, and can get notable
The rare earth luminescence of enhancing.
In the prior art, doping with rare-earth ions mayenite is prepared using coprecipitation；The technology, which still has, to be unable to get altogether
The technological deficiency of continuous hole structure and morphology.
Invention content
The technical problem to be solved in the present invention is to provide a kind of preparation methods of macropore mayenite fluorescent material, using the party
Method can obtain the doped rare earth element mayenite phosphor that pore-size is controllable, porosity is higher, with coherent macroporous structure
Material.
In order to solve the above technical problem, the present invention provides a kind of preparation methods of macropore mayenite fluorescent material, including
Following steps：
1) phase separation 0.02~0.12g of derivant, at room temperature, is dissolved in the mixed solvent, after magnetic agitation, then is added
Enter the Aluminium chloride hexahydrate (AlCl as presoma3·6H2O) 1.000~2.000g, CALCIUM CHLORIDE DIHYDRATE (CaCl2·2H2O)
Nine chloride hydrate terbium (TbCl of 0.400~1.044g and addition3·9H2O) 0.1~2.0g, 0.4 ± 0.1ml of drying control agent,
It is super to add 1.0~2.0ml of gel accelerating agent after stirring evenly (mixing time is 50~70min) by 0.3 ± 0.1ml of chelating agent
Sound 50~70 seconds；
2), the sol liquid (homogeneous transparent) obtained by step 1) is placed in closed container, in 50~70 DEG C of gels and old
Change 24 ± 2h；
3), gel after the ageing obtained by step 2) (white uniformity gel) is placed in container (non-closed container), and in
50~70 DEG C of dry 3~4d；Then it is heat-treated 2~3h in 900~1300 DEG C, obtains macropore mayenite fluorescent material (for crystallization
Doping Tb element macropore mayenites fluorescent material).
The improvement of the preparation method of macropore mayenite fluorescent material as the present invention：The mixed solvent is by 2 ± 0.2ml
Deionized water and 4 ± 0.4ml ethyl alcohol composition.
The preparation method of macropore mayenite fluorescent material as the present invention is further improved：Deionized water/ethyl alcohol=
1:2 volume ratio.
The preparation method of macropore mayenite fluorescent material as the present invention is further improved：The phase separation derivant
It is the polyethylene glycol oxide (PEO) that molecular weight is 300,000；Chelating agent is ethylene glycol (EG)；Gel accelerating agent be mass concentration be 24~
Ammonium hydroxide (the NH of 26% (being, for example, 25%)3H2O)；Drying control agent is formamide.
The preparation method of macropore mayenite fluorescent material as the present invention is further improved：In the step 1), gather
The dosage of ethylene oxide (PEO) is 0.04~0.08g, and mixed solvent is made of 2ml deionized waters and 4ml ethyl alcohol, mass concentration
Dosage for 25% ammonium hydroxide is 1.5ml.
The present invention is gone back while providing the macropore mayenite fluorescent material being prepared using any of the above-described method.
The step of temperature is not explicitly defined in the present invention carries out at room temperature, and room temperature refers to 10~30 DEG C.
The macropore mayenite fluorescent material of the present invention, using Aluminium chloride hexahydrate (AlCl3·6H2O), CALCIUM CHLORIDE DIHYDRATE
(CaCl2·2H2O), nine chloride hydrate terbium (TbCl3·9H2O), phase separation derivant, chelating agent, gel accelerating agent etc. are main
The mixture of raw material, deionized water and ethyl alcohol be solvent, by sol-gel be separated and combine heat treatment preparation by
At.
In the present invention, phase separation derivant can then be controlled with the separation of promotion system solid phase and liquid phase, gel accelerating agent
Gel time, to obtain the pattern in phase separation, the synergistic effect of the two can obtain corresponding construction and the hole of size
Structure.
There is coherent macroporous structure using mayenite fluorescent material prepared by this method, and can be lured by adjusting phase separation
The relative quantity of agent and gel accelerating agent is led to adjust macroporous structure, gained mayenite has stronger luminous intensity.
This method is simple for process, and raw material is easy to get, and greatly reduces the manufacturing cost of same type of material.
The collosol and gel of the present invention prepares the technique of macropore mayenite fluorescent material with phase separation method, uses system for chlorine
Salt is as presoma, and addition ammonium hydroxide is as gel accelerating agent on the basis of phase separation derivant and chelating agent is added, in phase point
From and collosol and gel during realize the formation and fixation of full penetrated macropore structure, and be successfully mixed with rare earth element.The party
Method prepares simple for process, and raw material is easy to get, at low cost, and the macropore mayenite luminous intensity of preparation is high, can be applied to fluorescent optical sensor
And the fields such as fluorescent powder.
Method using the present invention can go out the macropore mayenite block materials of rare earth doped Tb elements, macropore with one-step synthesis
Structure can make exciting light occur scattering and reflection, to reinforce the fluorescence intensity of visible light wave range, to obtain it is a kind of at
This cheap, good mayenite fluorescent material of luminous intensity.
The present invention uses terbium Tb3+As rear-earth-doped ion, and macropore is prepared with phase separation using sol-gel and mixes Tb
Mayenite fluorescent material obtains pore-size and can control, porosity is higher by control phase separation derivant and Tb dopings
The doped rare earth element mayenite fluorescent material with coherent macroporous structure.Macroporous structure can make exciting light occur scattering and
Reflection, to reinforce the fluorescence intensity of visible light wave range.
Description of the drawings
The specific implementation mode of the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is 2000 times of stereoscan photographs of macropore mayenite fluorescent material prepared by embodiment 1-1.
Fig. 2 is 2000 times of stereoscan photographs of macropore mayenite fluorescent material prepared by embodiment 1-2.
Fig. 3 is 2000 times of stereoscan photographs of macropore mayenite fluorescent material prepared by embodiment 1-3.
Fig. 4 is the fluorescence property that the PEO of different amounts prepares the macropore mayenite fluorescent material of gained.
Fig. 5 is the TbCl of different amounts3·9H2The fluorescence property of macropore mayenite fluorescent material prepared by O.
Specific implementation mode
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This.
Embodiment 1-1, a kind of preparation method of macropore mayenite block, follow the steps below successively：
1), at room temperature, will phase separation derivant polyethylene glycol oxide (PEO, molecular weight be 30 ten thousand) 0.04g be dissolved in
The in the mixed solvent of 2.0ml water and 4.0ml ethyl alcohol (alcohol) composition, after magnetic agitation, adds the 2.000g as presoma
Aluminium chloride hexahydrate (AlCl3·6H2O), 1.044g CALCIUM CHLORIDE DIHYDRATEs (CaCl2·2H2O), the nine chloride hydrate terbiums of 1g
(TbCl3·9H2O), and drying control agent (formamide) 0.4ml, chelating agent (ethylene glycol) 0.3ml stirring 60min is added, stirs
Mix uniformly after be added gel accelerating agent (a concentration of 25% ammonium hydroxide) 1.5ml and ultrasound 60 seconds；
2), the sol liquid of homogeneous transparent obtained by step 1) is placed in closed container, the gel and old in 70 DEG C of baking ovens
Change for 24 hours；
3), the white uniformity gel after the ageing obtained by step 2) is placed in non-closed container, and in 70 DEG C of environment
Dry 3~4d；Then 2h, the porous mayenite fluorescent material of doping Tb elements crystallized are heat-treated in 1100 DEG C.
Fig. 1 is 15000 times of lower stereoscan photographs of the macropore mayenite prepared, it can be seen that is continuously penetrated through in block is big
Hole (about 0.5 μm), porosity 78%.
The detection of the emission spectrum under 280nm excitation wavelengths is carried out to material, acquired results are with green light effect.
Embodiment 1-2,
By in embodiment 1-1 steps 1) phase separation derivant --- polyethylene glycol oxide makes 0.08g by 0.04g；Remaining is same
Embodiment 1-1.
Scanned Electronic Speculum low power and high power observation, the mayenite of gained still have a coherent macroporous structure simultaneously, but with
The increase of PEO amounts, macropore diameter are declined such as (Fig. 2, about 0.6 μm), porosity 72%.This is because PEO phase separations
Further progress.Through fluorometric investigation, luminous intensity is slightly decreased (such as Fig. 4).
Embodiment 1-3,
By in embodiment 1-1 steps 1) phase separation derivant --- polyethylene glycol oxide makes 0.12g by 0.04g；Remaining is same
Embodiment 1-1.
Scanned Electronic Speculum low power and high power observation, mayenite block microscopic appearance become mayenite particle packing and do not present
Coherent macroporous structure such as (Fig. 3), porosity 67%.This is because increasing with PEO amounts, PEO phase separations further increase
By force, there is excessive split-phase.Through fluorometric investigation, luminous intensity further declines (such as Fig. 4).
Embodiment 2-1,
By nine chloride hydrate terbium (TbCl in embodiment 1-1 steps 1)3·9H2O 0.8g) is made by 1g；Remaining is the same as implementation
Example 1-1.
Scanned Electronic Speculum low power and high power observation, after changing doping, the mayenite material of gained still has coherent simultaneously
Macroporous structure, aperture are about 0.5 μm, porosity 69%.Luminous intensity declines (such as Fig. 5).
Embodiment 2-2,
By nine chloride hydrate terbium (TbCl in embodiment 1-1 steps 1)3·9H2O 0.4g) is made by 1g；Remaining is the same as implementation
Example 1-1.
Scanned Electronic Speculum low power and high power observation, mayenite still has coherent macroporous structure, hole simultaneously after changing doping
Diameter is about 0.6 μm, porosity 67%.Luminous intensity further declines (such as Fig. 5).
Embodiment 2-3,
By nine chloride hydrate terbium (TbCl in embodiment 1-1 steps 1)3·9H2O 2.0g) is made by 1.0g；Remaining is the same as real
Apply a 1-1.
Be added after excessive terbium chloride system can not gel, final material cannot be obtained.
Comparative example 1,
Cancel terbium chloride (TbCl in embodiment 1-1 steps 1)3·9H2O use), that is, terbium chloride (TbCl3·9H2O)
Dosage 0g is made by 1g；Remaining is the same as embodiment 1-1.
There is no generate Fluorescent peal after tested for this sample.
Comparative example 2-1,
By phase separation in embodiment 1-1 steps 1), derivant --- the dosage of polyethylene glycol oxide makes 0 by 0.4g；Remaining is same
Embodiment 1-1.
Gained is transparent mayenite after the final drying of the present invention, this is because not having to be separated in system
Pore structure is generated, visible light can not be scattered, luminescent properties further decline.
Comparative example 2-2,
By the derivant that is separated in embodiment 1-1 steps 1) --- the molecular weight of polyethylene glycol oxide makes 10,000 by 300,000, uses
It measures constant；Remaining is equal to embodiment 1-1.Acquired results are：Enough phase separations do not occur, do not obtain co-continuous hole knot
Structure.
Comparative example 2-3,
By phase separation in embodiment 1-1 steps 1), derivant --- the molecular weight of polyethylene glycol oxide makes 1,000,000 by 300,000,
Dosage is constant；Remaining is equal to embodiment 1-1.Acquired results are：Obtain the structure and morphology of particle packing.
Nine chloride hydrate terbiums in embodiment 1-1 are made into terbium nitrate salt by comparative example 3, keep mole constant；Remaining etc.
It is same as
Embodiment 1-1.Acquired results are：It is unable to get the pattern of co-continuous pore space structure.
Comparative example 4 makes the ethylene glycol in embodiment 1-1 into citric acid, and volume is constant；Remaining is equal to embodiment 1-
1.Acquired results are：Back dissolving occurs for gel, can not normal gel.
Finally, it should also be noted that it is listed above be only the present invention several specific embodiments.Obviously, this hair
Bright to be not limited to above example, acceptable there are many deformations.Those skilled in the art can be from present disclosure
All deformations for directly exporting or associating, are considered as protection scope of the present invention.
Claims (9)
1. the preparation method of macropore mayenite fluorescent material, it is characterized in that including the following steps：
1) phase separation 0.02~0.12g of derivant, at room temperature, is dissolved in the mixed solvent, after magnetic agitation, adds work
For 1.000~2.000g of Aluminium chloride hexahydrate of presoma, 0.400~1.044g of CALCIUM CHLORIDE DIHYDRATE and nine hydration chlorine are added
Change 0.1~2.0g of terbium, 0.4 ± 0.1ml of drying control agent, 0.3 ± 0.1ml of chelating agent, after stirring evenly, adds gel promotion
1.0~2.0ml of agent ultrasounds 50~70 seconds；
2), the sol liquid obtained by step 1) is placed in closed container, in 50~70 DEG C of gels and is aged 24 ± 2h；
3), gel after the ageing obtained by step 2) is placed in container, and in 50~70 DEG C of dry 3~4d；Then in 900~
1300 DEG C of 2~3h of heat treatment, obtain macropore mayenite fluorescent material.
2. the preparation method of macropore mayenite fluorescent material according to claim 1, it is characterized in that：The mixed solvent by
2 ± 0.2ml deionized waters and 4 ± 0.4ml ethyl alcohol composition.
3. the preparation method of macropore mayenite fluorescent material according to claim 2, it is characterized in that：Deionized water/ethyl alcohol
=1:2 volume ratio.
4. according to the preparation method of any macropore mayenite fluorescent material of claims 1 to 3, it is characterized in that：
The phase separation derivant is the polyethylene glycol oxide that molecular weight is 300,000.
5. the preparation method of macropore mayenite fluorescent material according to claim 4, it is characterized in that：
Chelating agent is ethylene glycol.
6. the preparation method of macropore mayenite fluorescent material according to claim 5, it is characterized in that：
Gel accelerating agent is the ammonium hydroxide that mass concentration is 24~26%.
7. the preparation method of macropore mayenite fluorescent material according to claim 6, it is characterized in that：
Drying control agent is formamide.
8. the preparation method of macropore mayenite fluorescent material according to claim 7, it is characterized in that：
In the step 1), the dosage of polyethylene glycol oxide is 0.04~0.08g, and mixed solvent is by 2ml deionized waters and 4ml ethyl alcohol
Composition, the dosage for the ammonium hydroxide that mass concentration is 25% is 1.5ml.
9. the macropore mayenite fluorescent material being prepared using such as claim 1~8 either method.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109609120A (en) * | 2018-12-26 | 2019-04-12 | 同济大学 | A kind of long-persistence luminous aeroge and preparation method thereof |
| CN110157418A (en) * | 2019-05-16 | 2019-08-23 | 浙江大学 | It is used to prepare the preparation method of the porous mayenite fluorescent material of fluorescent optical sensor |
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| CN101538467A (en) * | 2009-04-07 | 2009-09-23 | 东北师范大学 | Method for preparing green light-emitting dodecacalcium heptaluminate powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109609120A (en) * | 2018-12-26 | 2019-04-12 | 同济大学 | A kind of long-persistence luminous aeroge and preparation method thereof |
| CN109609120B (en) * | 2018-12-26 | 2021-06-04 | 同济大学 | Long-afterglow luminescent aerogel and preparation method thereof |
| CN110157418A (en) * | 2019-05-16 | 2019-08-23 | 浙江大学 | It is used to prepare the preparation method of the porous mayenite fluorescent material of fluorescent optical sensor |
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