CN104358023A - Preparation method of Ca4Si2O7F2: Ce fluorescence fibrous membrane - Google Patents
Preparation method of Ca4Si2O7F2: Ce fluorescence fibrous membrane Download PDFInfo
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- CN104358023A CN104358023A CN201410521482.5A CN201410521482A CN104358023A CN 104358023 A CN104358023 A CN 104358023A CN 201410521482 A CN201410521482 A CN 201410521482A CN 104358023 A CN104358023 A CN 104358023A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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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
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7715—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing cerium
- C09K11/7719—Halogenides
- C09K11/772—Halogenides with alkali or alkaline earth metals
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
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Abstract
The invention relates to a preparation method of a Ca4Si2O7F2: Ce fluorescence fibrous membrane. The preparation method comprises the following steps: (1), adopting cerous nitrate, calcium nitrate, ammonium fluoride and TEOS as raw materials, adding the raw materials into a mixed solvent to obtain a uniformly mixed solution, adding polyvinylpyrrolidone to the solution, and stirring to obtain a transparent spinning solution; (2) performing electrostatic spinning to obtain an original fibrous membrane, and calcining the original fibrous membrane at 500-600 DEG C in an air atmosphere to obtain a precursor Ca-Si-O-F-Ce fibrous membrane; (3) raising the thermal treatment temperature to be 750-950 DEG C, and performing heat preservation for 1-3 h to obtain the Ca4Si2O7F2:Ce fluorescence fibrous membrane. The Ca4Si2O7F2: Ce fluorescence fibrous membrane is pure inorganic fluorescence fibrous membrane and can be applicable to remote packaging of high-power white light LED. The resultant temperature of the fluorescence fibrous membrane is lower, so that reaction energy consumption is reduced; in addition, the fluorescence fibrous membrane has certain mechanical strength, so that later packaging operation is facilitated.
Description
Technical field
The invention belongs to large power white light LED fluorescent material field, particularly a kind of Ca
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film.
Background technology
As lighting source of new generation, white light LEDs is to high efficiency and high-power future development.Because white light implementation general is at present the method utilizing blue chip to add yellow fluorophor conversion, the heat fade of light-emitting phosphor intensity becomes the bottleneck problem of restriction white light LEDs to high power development and large-scale promotion.Have except the fluorescent material system (as nitride) of more high thermal stability except finding, long-range another feasible way being encapsulated into solution large power white light LED light decay and look drift.
Be placed in reflector by fluorescent material in traditional packaged type, the utilizing emitted light of a part of luminescent powder faces toward chip and is absorbed by chip, cannot penetrate, cause light extraction efficiency not high at LED light direction.Particularly in great power LED field, due to dispel the heat bad more easily cause device temperature rising, light decay, look drift, homogeneity difference etc. problems.The Schubert research group of U.S. RensselaerPolytechnic Institute has developed a kind of long-range encapsulation technology (H.Luo et al.Appl.Phys.Lett., 2005,86:243505), by fluorescent material with excite chip to be separated by a distance, the efficiency theory utilizing reflector can make fluorescent material improves more than 50%.This kind of structure provides larger design freedom, more efficient production process and outstanding light quality, and also alleviates the impact of heating on light-emitting phosphor efficiency to a certain extent.
But LED long-distance fluorescent powder device is attached to by fluorescent material on substrate (normally silicon rubber) at present, separates with blue light LED light source, thus the heat that reduction chip produces is on the impact of light-emitting phosphor performance.But in great power LED, silicon rubber exists weather stain phenomenon equally, and the nitride (or oxynitride) of high temperature solid-state method synthesis is large due to particle diameter, reunites serious, and difficulty mixes with silicon rubber.
Have report to point out size uniform, the fluorescent fiber film luminescence of favorable dispersibility is better than simple fluorescent powder grain film (GYun et al.J.Mater.Chem., 2011,21:17790).But the fluorescent fiber film dynamic performance obtained is all lower, and heat treatment temperature is high.Crystallinity and optical property need further raising.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of Ca
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film, the method is prepared by electrostatic spinning technique can the precursor fibre film of low temperature calcination synthesis fluorescent material, and fibre structure reduce further the temperature of synthesis fluorescent material simultaneously.
A kind of Ca of the present invention
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film, comprising:
(1) preparation of spinning liquid as precursor:
With cerous nitrate, calcium nitrate, tetraethyl orthosilicate for raw material, join in mixed solvent; Add ammonium fluoride aqueous solution again in the solution mixed, stir the turbid liquid A obtaining calcium fluoride precipitate and produce; Polyvinylpyrrolidone is dissolved in ethanol, stirs and obtains clear solution B; Under agitation B solution is dropwise joined in A, mix and obtain transparent spinning solution;
(2) electrostatic spinning prepares protofibre film:
Under room temperature, above-mentioned spinning solution is adopted to carry out electrostatic spinning;
(3) preparation of precursor fibre film:
Tunica fibrosa is placed in be calcined in air atmosphere, is warming up to 500 ~ 600 DEG C, and insulation 2 ~ 4h, obtains presoma Ca-Si-O-F-Ce tunica fibrosa;
(4) heat treatment further:
After being down to room temperature, the presoma Ca-Si-O-F-Ce tunica fibrosa that obtains after step (3) calcining, continuing to pass in the atmosphere of ammonia or nitrogen and hydrogen mixture, is warming up to 750 ~ 950 DEG C, insulation 1 ~ 5h; Obtain Ca
4si
2o
7f
2: Ce fluorescent fiber film.
Cerous nitrate, calcium nitrate x in molar ratio in described step (1): (1-x) mixes, x=0.005 ~ 0.05.
Described step (1) middle Ca: Si=2 ~ 1.8: 1, Ca: F=2 ~ 1.8: 1.
In described step (1), ammonium fluoride aqueous solution concentration is 1.7mol/L, and mixed solvent is ultra-pure water and the absolute ethyl alcohol of volume ratio 1 ~ 2: 8.
NO in spinning solution in described step (1)
3 -concentration is 0.15mol/L ~ 0.4mol/L.
The PVP added in described step (1) is divided into two kinds, and the first molecular weight is 1300000, adds 0.8% ~ 1.2% of solution B quality, and the second molecular weight is 50000, adds 1.6% ~ 2.4% of solution B quality.
In described step (1), turbid liquid A and solution B volume ratio are 1: 0.8 ~ 1.
Spinning voltage 6-12kV, spinning speed 0.2-1.5mL/h in described step (2), receiving range 10-18cm, humid control is below 30%.
In described step (4), the flow velocity of ammonia or nitrogen and hydrogen mixture is 50-200mL/min, and the volume ratio of nitrogen and hydrogen is 95: 5.
In described step (3), heating rate is 1 ~ 2 DEG C/min, and in described step (4), heating rate is 2 ~ 3 DEG C/min.
beneficial effect
The present invention adopted electrostatic spinning technique to prepare first can low temperature calcination synthesis fluorescent material precursor fibre film, lower synthesis temperature makes tunica fibrosa have certain mechanical property, is conducive to the later stage encapsulation operation of white light LEDs.
Accompanying drawing explanation
Fig. 1. the Ca obtained after carrying out 1h heat treatment under different temperatures
4si
2o
7f
2: the emission spectrum of Ce fluorescent fiber film;
The Ca obtained after Fig. 2 .950 DEG C of heat treatment 1h
4si
2o
7f
2: the SEM photo of Ce fluorescent fiber film;
The Ca obtained after Fig. 3 .950 DEG C of heat treatment 1h
4si
2o
7f
2: the X-ray diffractogram of Ce fluorescent fiber film.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Get 1mL ultra-pure water and the mixing of 8mL absolute ethyl alcohol; By 0.009g cerous nitrate, 0.397g calcium nitrate is dissolved in mixed solvent, then adds 0.69mL TEOS.After Keep agitation 30min, slowly add the ammonium fluoride aqueous solution that 2mL concentration is 1.7mol/L under high velocity agitation, obtain the turbid liquid A that calcium fluoride precipitate produces.In 9mL ethanol, add 0.9g PVP (molecular weight 1300000) and 2.4g PVP (molecular weight 50000), continue to stir 3h, obtain clear solution B.Solution B is slowly joined in turbid liquid A, continue to stir 3h, obtain transparent spinning solution.
The precursor solution obtained is carried out electrostatic spinning: at room temperature, controlled humidity is 30%, and spinning voltage is set to 6kv, and the fltting speed of boost pump is 0.2mL/h, and receiving range is 10cm.
In air atmosphere, calcine as-spun fibre obtained above, heating rate is 0.8 DEG C/min, and calcining heat 500 DEG C is, Temperature fall after insulation 4h, obtains presoma Ca-Si-O-F-Ce tunica fibrosa.
Tunica fibrosa after calcining is transferred to tube-type atmosphere furnace, and pass into nitrogen and hydrogen mixture (95: 5), throughput is 200mL/min, the heating rate of tube-type atmosphere furnace is 3 DEG C/min, is warming up to 750 DEG C, and is incubated 5h, under flowing nitrogen and hydrogen mixture, be cooled to room temperature, obtain Ca
4si
2o
7f
2: Ce fluorescent fiber film.
Embodiment 2
Get 1.5mL ultra-pure water and the mixing of 8mL absolute ethyl alcohol; By 0.019g cerous nitrate, 0.624g calcium nitrate is dissolved in mixed solvent, then adds 1.03mL TEOS.After Keep agitation 30min, slowly add the ammonium fluoride aqueous solution that 3mL concentration is 1.7mol/L under high velocity agitation, obtain the turbid liquid A that calcium fluoride precipitate produces.In 9mL ethanol, add 1g PVP (molecular weight 1300000) and 2g PVP (molecular weight 50000), continue to stir 3h, obtain clear solution B.Solution B is slowly joined in turbid liquid A, continue to stir 3h, obtain transparent spinning solution.
The precursor solution obtained is carried out electrostatic spinning: at room temperature, controlled humidity is 30%, and spinning voltage is set to 8kv, and the fltting speed of boost pump is 0.8mL/h, and receiving range is 14cm.
In air atmosphere, calcine as-spun fibre obtained above, heating rate is 1 DEG C/min, and calcining heat 550 DEG C is, Temperature fall after insulation 3h, obtains presoma Ca-Si-O-F-Ce tunica fibrosa.
Tunica fibrosa after calcining is transferred to tube-type atmosphere furnace, and pass into nitrogen and hydrogen mixture (95: 5), throughput is 100mL/min, the heating rate of tube-type atmosphere furnace is 3 DEG C/min, is warming up to 850 DEG C, and is incubated 3h, under flowing nitrogen and hydrogen mixture, be cooled to room temperature, obtain Ca
4si
2o
7f
2: Ce fluorescent fiber film.
Embodiment 3
Get 2mL ultra-pure water and the mixing of 8mL absolute ethyl alcohol; By 0.031g cerous nitrate, 0.932g calcium nitrate is dissolved in mixed solvent, then adds 1.48mL TEOS.After Keep agitation 30min, slowly add the ammonium fluoride aqueous solution that 4.8mL concentration is 1.7mol/L under high velocity agitation, obtain the turbid liquid A that calcium fluoride precipitate produces.In 9mL ethanol, add 1.2g PVP (molecular weight 1300000) and 1.7g PVP (molecular weight 50000), continue to stir 3h, obtain clear solution B.Solution B is slowly joined in turbid liquid A, continue to stir 3h, obtain transparent spinning solution.
The precursor solution obtained is carried out electrostatic spinning: at room temperature, controlled humidity is 30%, and spinning voltage is set to 12kv, and the fltting speed of boost pump is 1.5mL/h, and receiving range is 18cm.
In air atmosphere, calcine as-spun fibre obtained above, heating rate is 1.5 DEG C/min, and calcining heat 600 DEG C is, Temperature fall after insulation 2h, obtains presoma Ca-Si-O-F-Ce tunica fibrosa.
Tunica fibrosa after calcining is transferred to tube-type atmosphere furnace, and pass into nitrogen and hydrogen mixture (95: 5), throughput is 50mL/min, the heating rate of tube-type atmosphere furnace is 3 DEG C/min, is warming up to 950 DEG C, and is incubated 1h, under flowing nitrogen and hydrogen mixture, be cooled to room temperature, obtain Ca
4si
2o
7f
2: Ce fluorescent fiber film.
Claims (10)
1. a Ca
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film, comprising:
(1) with cerous nitrate, calcium nitrate, tetraethyl orthosilicate for raw material, join in mixed solvent; Add ammonium fluoride aqueous solution again in the solution mixed, stir the turbid liquid A obtaining calcium fluoride precipitate and produce; Polyvinylpyrrolidone is dissolved in ethanol, stirs and obtains clear solution B; Under agitation B solution is dropwise joined in A, mix and obtain transparent spinning solution;
(2), under room temperature, above-mentioned spinning solution is adopted to carry out electrostatic spinning;
(3) tunica fibrosa is placed in and calcines in air atmosphere, is warming up to 500 ~ 600 DEG C, and insulation 2 ~ 4h, obtains presoma Ca-Si-O-F-Ce tunica fibrosa;
(4), after being down to room temperature, the presoma Ca-Si-O-F-Ce tunica fibrosa that obtains after step (3) calcining, continuing to pass in the atmosphere of ammonia or nitrogen and hydrogen mixture, is warming up to 750 ~ 950 DEG C, insulation 1 ~ 5h; Obtain Ca
4si
2o
7f
2: Ce fluorescent fiber film.
2. a kind of Ca as claimed in claim 1
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film, is characterized in that: cerous nitrate, calcium nitrate x in molar ratio in described step (1): (1-x) mixes, x=0.005 ~ 0.05.
3. a kind of Ca as claimed in claim 1
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film, is characterized in that: described step (1) middle Ca: Si=2 ~ 1.8: 1, Ca: F=2 ~ 1.8: 1.
4. a kind of Ca as claimed in claim 1
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film, is characterized in that: in described step (1), ammonium fluoride aqueous solution concentration is 1.7mol/L, and mixed solvent is ultra-pure water and the absolute ethyl alcohol of volume ratio 1 ~ 2: 8.
5. a kind of Ca as claimed in claim 1
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film, is characterized in that: NO in spinning solution in described step (1)
3 -concentration is 0.15mol/L ~ 0.4mol/L.
6. a kind of Ca as claimed in claim 1
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film, it is characterized in that: the PVP added in described step (1) is divided into two kinds, and the first molecular weight is 1300000, adds 0.8% ~ 1.2% of solution B quality, the second molecular weight is 50000, adds 1.6% ~ 2.4% of solution B quality.
7. a kind of Ca as claimed in claim 1
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film, is characterized in that: in described step (1), turbid liquid A and solution B volume ratio are 1: 0.8 ~ 1.
8. a kind of Ca as claimed in claim 1
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film, is characterized in that: spinning voltage 6-12kV, spinning speed 0.2-1.5mL/h in described step (2), receiving range 10-18cm, humid control is below 30%.
9. a kind of Ca as claimed in claim 1
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film, is characterized in that: in described step (4), the flow velocity of ammonia or nitrogen and hydrogen mixture is 50-200mL/min, and the volume ratio of nitrogen and hydrogen is 95: 5.
10. a kind of Ca as claimed in claim 1
4si
2o
7f
2: the preparation method of Ce fluorescent fiber film, is characterized in that: in described step (3), heating rate is 1 ~ 2 DEG C/min, and in described step (4), heating rate is 2 ~ 3 DEG C/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106206873A (en) * | 2016-08-08 | 2016-12-07 | 雷春生 | A kind of preparation method of high light efficiency LED lamp flourescent sheet |
| CN110938427A (en) * | 2019-11-29 | 2020-03-31 | 湖北大学 | Rare earth metal doped alkaline earth metal silicate material, preparation method and application thereof, and light-emitting device |
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2014
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| CN106206873A (en) * | 2016-08-08 | 2016-12-07 | 雷春生 | A kind of preparation method of high light efficiency LED lamp flourescent sheet |
| CN110938427A (en) * | 2019-11-29 | 2020-03-31 | 湖北大学 | Rare earth metal doped alkaline earth metal silicate material, preparation method and application thereof, and light-emitting device |
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