CN104358028A - A method for preparing white light emitting Ca4Si2O7F2: ce, tb, sm fluorescent fiber film - Google Patents

A method for preparing white light emitting Ca4Si2O7F2: ce, tb, sm fluorescent fiber film Download PDF

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Publication number
CN104358028A
CN104358028A CN201410521468.5A CN201410521468A CN104358028A CN 104358028 A CN104358028 A CN 104358028A CN 201410521468 A CN201410521468 A CN 201410521468A CN 104358028 A CN104358028 A CN 104358028A
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white light
preparation
fiber film
fluorescent fiber
light emission
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CN201410521468.5A
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CN104358028B (en
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王宏志
崔博
李耀刚
张青红
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Donghua University
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Donghua University
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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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/02—Preparation of spinning solutions
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • 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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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention relates to a preparation method of a white-light-emissive Ca4Si2O7F2: Ce, Tb, Sm 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, adding polyvinylpyrrolidone, 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; (3) performing calcining in an ammonia gas or nitrogen- hydrogen mixed gas atmosphere at 750-950 DEG C, and performing heat preservation for 1-3 h to obtain the white-light-emissive Ca4Si2O7F2: Ce, Tb, Sm fluorescence fibrous membrane. The preparation method of the white-light-emissive Ca4Si2O7F2: Ce, Tb, Sm fluorescence fibrous membrane is applicable to remote packaging of high-power white light LED. White light emission solves the later color matching problem of an LED and simplifies the technology. The resultant temperature of the fluorescence fibrous membrane is lower, so that reaction energy consumption is reduced.

Description

A kind of Ca of white light emission 4si 2o 7f 2: the preparation method of Ce, Tb, Sm fluorescent fiber film
Technical field
The invention belongs to large power white light LED fluorescent material, particularly a kind of Ca of white light emission 4si 2o 7f 2: the preparation method of Ce, Tb, Sm 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.
The Schubert research group of U.S. Rensselaer Polytechnic 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.For the packaged type that this is new, industrial circle is active response also, such as PHILIPS Co. (Philips) is proposed Fortimo remote fluorescence component powder in international light fixture exhibition in 2008, and famous Intematix company of fluorescent material supplier has also issued ChromaLit long-distance fluorescent powder light source in January, 2011.
Current business-like remote fluorescence component powder is that fluorescent material is mixed film forming with silicon rubber (or resin), and attachment on the transparent substrate, is then encapsulated in the top of LED chip reflector.Such as, but along with the LED power of research and development constantly promotes, the illumination life-span constantly extends, and fluorescent material also manifests gradually with the shortcoming of silicon rubber mixing thin film-forming method: the problem of aging of silicon rubber; The scattering problem of fluorescent powder in silica gel.Particularly there is multiple fluorescent material in high color rendering index (CRI) fluorescent material, their dispersed direct uniformity affecting light source luminescent.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of Ca of white light emission 4si 2o 7f 2: the preparation method of Ce, Tb, Sm fluorescent fiber film, the method is dispersed by different rare earth ions by electrostatic spinning technique, and fluorescent fiber luminescence is homogeneous.Tunica fibrosa possesses white light emission performance, without the need to color matching in LED, and Simplified flowsheet.
The Ca of a kind of white light emission of the present invention 4si 2o 7f 2: the preparation method of Ce, Tb, Sm fluorescent fiber film, comprising:
(1) preparation of spinning liquid as precursor:
With cerous nitrate, terbium nitrate, samaric 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 high velocity 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-Tb-Sm tunica fibrosa;
(4) heat treatment further:
After being down to room temperature, the presoma Ca-Si-O-F-Ce-Tb-Sm 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, and insulation 1 ~ 5h, obtains Ca 4si 2o 7f 2: Ce, Tb, Sm fluorescent fiber film.
In described step (1) in molar ratio, Ca: Ce=1: 0.001 ~ 0.01, Ce: Tb=1: 0.5 ~ 1, Ce: Sm=1: 2 ~ 5, Ca: Si=2 ~ 1.8: 1, Ca: F=2 ~ 1.8: 1.
In described step (1), mixed solvent is ultra-pure water and the absolute ethyl alcohol of volume ratio 1 ~ 2: 8.
In described step (1), the concentration of ammonium fluoride aqueous solution is 1.7mol/L.
Spinning solution NO 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), the volume ratio of turbid liquid A and solution B is 1: 0.8 ~ 1.
Described step (2) spinning technology parameter is voltage 6-12kV, spinning speed 0.2-1.5mL/h, and receiving range 10-18cm, humid control is below 30%.
In described step (4) ammonia or flow velocity be 50-200mL/min, in nitrogen and hydrogen mixture, nitrogen and hydrogen volume ratio are 95: 5.
Heating rate 1 ~ 2 DEG C/min in described step (3), heating rate 2 ~ 3 DEG C/min in described step (4).
beneficial effect
First passage electrostatic spinning technique of the present invention has prepared the fluorescent nano-fiber film with white light emission performance, and fluorescent fiber film luminescence is homogeneous, without the need to color matching in LED, simplifies packaging technology.
Accompanying drawing explanation
The Ca with white light emission obtained after Fig. 1 .950 DEG C of heat treatment 1h 4si 2o 7f 2: the emission spectrum of Ce, Tb, Sm fluorescent fiber film;
The Ca with white light emission obtained after Fig. 2 .950 DEG C of heat treatment 1h 4si 2o 7f 2: the SEM photo of Ce, Tb, Sm fluorescent fiber film;
The Ca with white light emission obtained after Fig. 3 .800 DEG C of heat treatment 2h 4si 2o 7f 2: the X-ray diffractogram of Ce, Tb, Sm 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, 0.009g terbium nitrate, 0.023g samaric 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 10em.
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-Tb-Sm 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, Tb, Sm fluorescent fiber film.
Embodiment 2
Get 1.5mL ultra-pure water and the mixing of 8mL absolute ethyl alcohol; By 0.019g cerous nitrate, 0.012g terbium nitrate, 0.093g samaric 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 14em.
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-Tb-Sm 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, Tb, Sm fluorescent fiber film.
Embodiment 3
Get 2mL ultra-pure water and the mixing of 8mL absolute ethyl alcohol; By 0.031g cerous nitrate, 0.015g terbium nitrate, 0.123g samaric 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 18em.
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-Tb-Sm 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, Tb, Sm fluorescent fiber film.

Claims (10)

1. the Ca of a white light emission 4si 2o 7f 2: the preparation method of Ce, Tb, Sm fluorescent fiber film, comprising:
(1) with cerous nitrate, terbium nitrate, samaric 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 high velocity 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-Tb-Sm tunica fibrosa;
(4), after being down to room temperature, the presoma Ca-Si-O-F-Ce-Tb-Sm 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, and insulation 1 ~ 5h, obtains Ca 4si 2o 7f 2: Ce, Tb, Sm fluorescent fiber film.
2. the Ca of a kind of white light emission according to claim 1 4si 2o 7f 2: the preparation method of Ce, Tb, Sm fluorescent fiber film, it is characterized in that: in described step (1) in molar ratio, Ca: Ce=1: 0.001 ~ 0.01, Ce: Tb=1: 0.5 ~ 1, Ce: Sm=1: 2 ~ 5, Ca: Si=2 ~ 1.8: 1, Ca: F=2 ~ 1.8: 1.
3. the Ca of a kind of white light emission according to claim 1 4si 2o 7f 2: the preparation method of Ce, Tb, Sm fluorescent fiber film, is characterized in that: in described step (1), mixed solvent is ultra-pure water and the absolute ethyl alcohol of volume ratio 1 ~ 2: 8.
4. the Ca of a kind of white light emission according to claim 1 4si 2o 7f 2: the preparation method of Ce, Tb, Sm fluorescent fiber film, is characterized in that: in described step (1), the concentration of ammonium fluoride aqueous solution is 1.7mol/L.
5. the Ca of a kind of white light emission according to claim 1 4si 2o 7f 2: the preparation method of Ce, Tb, Sm fluorescent fiber film, is characterized in that: spinning solution NO in described step (1) 3 -concentration is 0.15mol/L ~ 0.4mol/L.
6. the Ca of a kind of white light emission according to claim 1 4si 2o 7f 2: Ce, Tb, the preparation method of Sm fluorescent fiber film, it is characterized in that: the PVP added in described step (1) is divided into two kinds, the first molecular weight is 1300000, add 0.8% ~ 1.2% of solution B quality, the second molecular weight is 50000, adds 1.6% ~ 2.4% of solution B quality.
7. the Ca of a kind of white light emission according to claim 1 4si 2o 7f 2: the preparation method of Ce, Tb, Sm fluorescent fiber film, is characterized in that: in described step (1), the volume ratio of turbid liquid A and solution B is 1: 0.8 ~ 1.
8. the Ca of a kind of white light emission according to claim 1 4si 2o 7f 2: the preparation method of Ce, Tb, Sm fluorescent fiber film, is characterized in that: described step (2) spinning technology parameter is voltage 6-12kV, spinning speed 0.2-1.5mL/h, and receiving range 10-18cm, humid control is below 30%.
9. the Ca of a kind of white light emission according to claim 1 4si 2o 7f 2: the preparation method of Ce, Tb, Sm fluorescent fiber film, is characterized in that: in described step (4) ammonia or flow velocity be 50-200mL/min, in nitrogen and hydrogen mixture, nitrogen and hydrogen volume ratio are 95: 5.
10. the Ca of a kind of white light emission according to claim 1 4si 2o 7f 2: the preparation method of Ce, Tb, Sm fluorescent fiber film, is characterized in that: heating rate 1 ~ 2 DEG C/min in described step (3), heating rate 2 ~ 3 DEG C/min in described step (4).
CN201410521468.5A 2014-09-30 A kind of Ca of white light emission4si2o7f2: the preparation method of Ce, Tb, Sm fluorescent fiber film Expired - Fee Related CN104358028B (en)

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Citations (4)

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JP2000212360A (en) * 1999-01-27 2000-08-02 Asahi Glass Co Ltd Fluororesin composition for coating fluorescent lamp, coating material and fluorescent lamp
EP2275505A1 (en) * 2009-06-05 2011-01-19 Xerox Corporation Hydrophobic coatings and their processes
CN101962823A (en) * 2010-09-29 2011-02-02 黑龙江大学 PH color response sensing micro-nano fiber, preparation method and application thereof
CN103088554A (en) * 2011-10-31 2013-05-08 中国科学院合肥物质科学研究院 Porous membrane mixed by 1,4-dihydroxy anthraquinone and cellulose, preparation method and usage

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000212360A (en) * 1999-01-27 2000-08-02 Asahi Glass Co Ltd Fluororesin composition for coating fluorescent lamp, coating material and fluorescent lamp
EP2275505A1 (en) * 2009-06-05 2011-01-19 Xerox Corporation Hydrophobic coatings and their processes
CN101962823A (en) * 2010-09-29 2011-02-02 黑龙江大学 PH color response sensing micro-nano fiber, preparation method and application thereof
CN103088554A (en) * 2011-10-31 2013-05-08 中国科学院合肥物质科学研究院 Porous membrane mixed by 1,4-dihydroxy anthraquinone and cellulose, preparation method and usage

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* Cited by examiner, † Cited by third party
Title
丁狄等: "静电纺丝制备La3Si8O4N11:Ln（Ce3+,Sm3+）纳米纤维及其发光性能研究", 《无机材料学报》 *

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