CN106517774A - Preparation method of white-light-emitting glass material - Google Patents
Preparation method of white-light-emitting glass material Download PDFInfo
- Publication number
- CN106517774A CN106517774A CN201611225997.6A CN201611225997A CN106517774A CN 106517774 A CN106517774 A CN 106517774A CN 201611225997 A CN201611225997 A CN 201611225997A CN 106517774 A CN106517774 A CN 106517774A
- Authority
- CN
- China
- Prior art keywords
- white light
- glass material
- preparation
- light emitting
- emitting glass
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
Abstract
The invention belongs to the technical field of glass and particularly relates to a preparation method of a white-light-emitting glass material. The preparation method includes the steps of firstly, weighing raw materials according to weight; secondly, performing ball milling, drying, sieving and melting to obtain even glass liquid; thirdly, performing fast casting molding on the glass liquid, annealing, and cooling to room temperature to obtain the white-light-emitting glass material. The preparation method has the advantages that the method is simple in process, easy to operate, free of pollution and low in cost, and the prepared white-light-emitting glass material can emit a series of slightly-red and slightly-blue white light and pure-white light and is stable in performance, high in light emitting efficiency and color rendering index, and the like.
Description
Technical field
The invention belongs to glass technology field, more particularly to a kind of preparation method of white light emitting glass material.
Background technology
Quasiconductor white light-emitting diode (light-emitting diodes, abbreviation LED) is closely to develop during the last ten years
A kind of New Solid illuminating device for coming.Compared with traditional electric filament lamp, fluorescent lamp, white light LEDs have energy-conservation, efficiency high, little
Type solidification, vibration resistance are hardly damaged, instantaneous starting and quick response, energy-conservation and life-span length, environmental friendliness, Color tunable etc.
Advantage, is referred to as " forth generation lighting source ".At present, conventional white light LEDs need to using organic resin by blue-light LED chip with
YAG:Ce fluorescent powder packagings get up.But the organic resin of encapsulation is easily aging, obtains in particular by ultraviolet leds chip
In the scheme of white light LEDs, the life-span of device substantially reduces, and develops a kind of new material solving these problems and has important meaning
Justice.
Traditional business-like most of White-light LED illumination device uses blue light for InGaN chip and is excited by blue light
Send yellow, green or orange fluorescent material.This kind of fluorescent material has higher luminous efficiency, ripe preparation method etc. excellent
Point.But while also there is following defect：(1) fluorescent material is different with the aging rate of decay of chip, so as to result in chromaticity coordinates
Unstable, white light easily drifts about；(2) as the epoxy resin or silica gel for encapsulation is subject to blue light or ultraviolet for a long time
Radiate and cause epoxy resin or the easy aging yellowing of silica gel unstable, device lifetime reduces；(3) encapsulating material is expensive, leads
Cause high cost.Simultaneously because white light is formed with the blue light of LED by the yellow fluorescence of fluorophor, the glow color of device with
The change of driving voltage and fluorescent coating thickness and change, color reducibility is poor, and color rendering index is low.To solve the above problems,
Panchromatic single-substrate white glass can overcome the shortcomings of mixing phosphor to a certain extent, improve luminous efficiency and colour developing refers to
Number；And resin is substituted by glass and can also optimize packaging technology.
Therefore the efficient single-substrate white glass for developing suitable burst of ultraviolel has wide Economic Application value.
The content of the invention
The technical problem to be solved is to provide a kind of stable performance, the high white light of luminous efficiency and color rendering index
Luminous glass material.
For achieving the above object, the present invention is adopted the following technical scheme that：
The present invention provides a kind of preparation method of white light emitting glass material, including following preparation process：
1) raw material is weighed according to following weight portion：20～38 parts of silicon dioxide, 10～22 parts of calcium oxide, aluminium oxide 8～20
Part, 1～7 part of sodium phosphate, 0.03～0.15 part of lithium carbonate, 0.02～0.08 part of Disamarium trioxide；
2) ball milling, drying, sieves, and is incubated 40～70min at 1050 DEG C～1100 DEG C and is melting into uniform glass liquid；
3) the rapid moulding by casting of vitreous humour, is cooled to room after being then incubated 4～8h in 550 DEG C～580 DEG C of annealing furnace
Temperature, obtains white light emitting glass material.
Preferably, the preparation method of white light emitting glass material of the present invention, the step 1) in, according to following heavy
Amount part weighs raw material：29 parts of silicon dioxide, 16 parts of calcium oxide, 14 parts of aluminium oxide, 4 parts of sodium phosphate, 0.09 part of lithium carbonate, Disamarium trioxide
0.05 part.
Preferably, step 2 of the present invention) in, 12～24h of ball milling.Ball-milling Time ensure that the particle diameter of raw material.
Preferably, step 2 of the present invention) in, cross 100 mesh sieves.
Preferably, step 2 of the present invention) in, heating rate is 18～24 DEG C/min.It is rapidly heated in this speed,
The bulk density of white light emitting glass material is significantly improved, sintering activation energy, stomatal frequency and pore size is reduced, is significantly improved
The bending strength of white light emitting glass material.
Preferably, step 2 of the present invention) in, it is incubated at 1080 DEG C, insulation at such a temperature is founded, it is ensured that white
The stability of light luminous glass material.
Preferably, step 3 of the present invention) in, with 3～6 DEG C/min ramps.
Whole material purities of the present invention are up to more than 99%.
The beneficial effects of the present invention is：
1st, the preparation method process is simple of white light emitting glass material of the invention, it is easy to operate, pollution-free, low cost.
2nd, the white light emitting glass material that the inventive method is prepared can launch partially red, the partially blue white light of series and
Positive white light, color rendering index is up to more than 93.
3rd, the white light emitting glass material that the inventive method is prepared has stable performance, the advantages of luminous efficiency is high.
Specific embodiment
The invention will be further described with reference to embodiments, but the invention is not limited in these embodiments.
Embodiment 1
A kind of preparation method of white light emitting glass material, including following preparation process：
1) raw material is weighed according to following weight portion：20 parts of silicon dioxide, 22 parts of calcium oxide, 8 parts of aluminium oxide, 7 parts of sodium phosphate,
0.03 part of lithium carbonate, 0.08 part of Disamarium trioxide；
2), in adding dehydrated alcohol, with zirconia ball ball milling 12h, dry, cross 100 mesh sieves, with 24 DEG C/min ramps
1050 DEG C, insulation 70min is melting into uniform glass liquid；
3) the rapid moulding by casting of vitreous humour, it is then cold after 4h to be incubated in the annealing furnace of 3 DEG C/min ramps to 580 DEG C
But to room temperature, obtain white light emitting glass material.
Product Jing is tested：White light emitting glass material is in the chromaticity coordinates that wavelength is glass sample under 377nm ultraviolet excitations
(x, y) for (0.316,0.324), be in close proximity to standard illuminants white light (x=0.333, y=0.333)；Bending strength
108Mpa。
Embodiment 2
A kind of preparation method of white light emitting glass material, including following preparation process：
1) raw material is weighed according to following weight portion：23 parts of silicon dioxide, 20 parts of calcium oxide, 10 parts of aluminium oxide, sodium phosphate 6
Part, 0.05 part of lithium carbonate, 0.07 part of Disamarium trioxide；
2), in adding dehydrated alcohol, with zirconia ball ball milling 14h, dry, cross 100 mesh sieves, with 23 DEG C/min ramps
1060 DEG C, insulation 65min is melting into uniform glass liquid；
3) the rapid moulding by casting of vitreous humour, it is then cold after 6h to be incubated in the annealing furnace of 4 DEG C/min ramps to 570 DEG C
But to room temperature, obtain white light emitting glass material.
Product Jing is tested：White light emitting glass material is in the chromaticity coordinates that wavelength is glass sample under 377nm ultraviolet excitations
(x, y) for (0.328,0.325), be in close proximity to standard illuminants white light (x=0.333, y=0.333)；Bending strength
100Mpa。
Embodiment 3
A kind of preparation method of white light emitting glass material, including following preparation process：
1) raw material is weighed according to following weight portion：26 parts of silicon dioxide, 18 parts of calcium oxide, 12 parts of aluminium oxide, sodium phosphate 5
Part, 0.07 part of lithium carbonate, 0.06 part of Disamarium trioxide；
2), in adding dehydrated alcohol, with zirconia ball ball milling 16h, dry, cross 100 mesh sieves, with 22 DEG C/min ramps
1070 DEG C, insulation 60min is melting into uniform glass liquid；
3) the rapid moulding by casting of vitreous humour, it is then cold after 8h to be incubated in the annealing furnace of 5 DEG C/min ramps to 565 DEG C
But to room temperature, obtain white light emitting glass material.
Product Jing is tested：White light emitting glass material is in the chromaticity coordinates that wavelength is glass sample under 377nm ultraviolet excitations
(x, y) for (0.326,0.346), be in close proximity to standard illuminants white light (x=0.333, y=0.333)；Bending strength 95Mpa.
Embodiment 4
A kind of preparation method of white light emitting glass material, including following preparation process：
1) raw material is weighed according to following weight portion：29 parts of silicon dioxide, 16 parts of calcium oxide, 14 parts of aluminium oxide, sodium phosphate 4
Part, 0.09 part of lithium carbonate, 0.05 part of Disamarium trioxide；
2), in adding dehydrated alcohol, with zirconia ball ball milling 18h, dry, cross 100 mesh sieves, with 21 DEG C/min ramps
1080 DEG C, insulation 55min is melting into uniform glass liquid；
3) the rapid moulding by casting of vitreous humour, it is then cold after 7h to be incubated in the annealing furnace of 4 DEG C/min ramps to 560 DEG C
But to room temperature, obtain white light emitting glass material.
Product Jing is tested：White light emitting glass material is in the chromaticity coordinates that wavelength is glass sample under 377nm ultraviolet excitations
(x, y) for (0.332,0.332), be in close proximity to standard illuminants white light (x=0.333, y=0.333)；Bending strength
105Mpa。
Embodiment 5
A kind of preparation method of white light emitting glass material, including following preparation process：
1) raw material is weighed according to following weight portion：32 parts of silicon dioxide, 14 parts of calcium oxide, 16 parts of aluminium oxide, sodium phosphate 3
Part, 0.11 part of lithium carbonate, 0.04 part of Disamarium trioxide；
2), in adding dehydrated alcohol, with zirconia ball ball milling 20h, dry, cross 100 mesh sieves, with 20 DEG C/min ramps
1090 DEG C, insulation 50min is melting into uniform glass liquid；
3) the rapid moulding by casting of vitreous humour, it is then cold after 6h to be incubated in the annealing furnace of 5 DEG C/min ramps to 555 DEG C
But to room temperature, obtain white light emitting glass material.
Product Jing is tested：White light emitting glass material is in the chromaticity coordinates that wavelength is glass sample under 358nm ultraviolet excitations
(x, y) for (0.329,0.330), be in close proximity to standard illuminants white light (x=0.333, y=0.333)；Bending strength
103Mpa。
Embodiment 6
A kind of preparation method of white light emitting glass material, including following preparation process：
1) raw material is weighed according to following weight portion：35 parts of silicon dioxide, 12 parts of calcium oxide, 18 parts of aluminium oxide, sodium phosphate 2
Part, 0.13 part of lithium carbonate, 0.03 part of Disamarium trioxide；
2), in adding dehydrated alcohol, with zirconia ball ball milling 22h, dry, cross 100 mesh sieves, with 19 DEG C/min ramps
1100 DEG C, insulation 45min is melting into uniform glass liquid；
3) the rapid moulding by casting of vitreous humour, it is then cold after 5h to be incubated in the annealing furnace of 6 DEG C/min ramps to 550 DEG C
But to room temperature, obtain white light emitting glass material.
Product Jing is tested：White light emitting glass material is in the chromaticity coordinates that wavelength is glass sample under 377nm ultraviolet excitations
(x, y) for (0.328,0.319), be in close proximity to standard illuminants white light (x=0.333, y=0.333)；Bending strength
105Mpa。
Embodiment 7
A kind of preparation method of white light emitting glass material, including following preparation process：
1) raw material is weighed according to following weight portion：38 parts of silicon dioxide, 10 parts of calcium oxide, 20 parts of aluminium oxide, sodium phosphate 1
Part, 0.15 part of lithium carbonate, 0.02 part of Disamarium trioxide；
2), in adding dehydrated alcohol, with zirconia ball ball milling 24h, dry, cross 100 mesh sieves, with 18 DEG C/min ramps
1080 DEG C, insulation 40min is melting into uniform glass liquid；
3) the rapid moulding by casting of vitreous humour, it is then cold after 4h to be incubated in the annealing furnace of 3 DEG C/min ramps to 575 DEG C
But to room temperature, obtain white light emitting glass material.
Product Jing is tested：White light emitting glass material is in the chromaticity coordinates that wavelength is glass sample under 377nm ultraviolet excitations
(x, y) for (0.332,0.329), be in close proximity to standard illuminants white light (x=0.333, y=0.333)；Bending strength
101Mpa。
Claims (7)
1. a kind of preparation method of white light emitting glass material, it is characterised in that including following preparation process：
1) raw material is weighed according to following weight portion：20～38 parts of silicon dioxide, 10～22 parts of calcium oxide, 8～20 parts of aluminium oxide, phosphorus
1～7 part of sour sodium, 0.03～0.15 part of lithium carbonate, 0.02～0.08 part of Disamarium trioxide；
2) ball milling, drying, sieves, and is incubated 40～70min at 1050 DEG C～1100 DEG C and is melting into uniform glass liquid；
3) the rapid moulding by casting of vitreous humour, is cooled to room temperature after being then incubated 4～8h in 550 DEG C～580 DEG C of annealing furnace, obtains
To white light emitting glass material.
2. the preparation method of white light emitting glass material according to claim 1, it is characterised in that the step 1) in,
Raw material is weighed according to following weight portion：29 parts of silicon dioxide, 16 parts of calcium oxide, 14 parts of aluminium oxide, 4 parts of sodium phosphate, lithium carbonate
0.09 part, 0.05 part of Disamarium trioxide.
3. the preparation method of white light emitting glass material according to claim 1, it is characterised in that：The step 2) in,
12～24h of ball milling.
4. the preparation method of white light emitting glass material according to claim 1, it is characterised in that：The step 2) in,
Cross 100 mesh sieves.
5. the preparation method of white light emitting glass material according to claim 1, it is characterised in that：The step 2) in,
Heating rate is 18～24 DEG C/min.
6. the preparation method of white light emitting glass material according to claim 1, it is characterised in that：The step 2) in,
It is incubated at 1080 DEG C.
7. the preparation method of white light emitting glass material according to claim 1, it is characterised in that：The step 3) in,
With 3～6 DEG C/min ramps.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611225997.6A CN106517774A (en) | 2016-12-27 | 2016-12-27 | Preparation method of white-light-emitting glass material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611225997.6A CN106517774A (en) | 2016-12-27 | 2016-12-27 | Preparation method of white-light-emitting glass material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106517774A true CN106517774A (en) | 2017-03-22 |
Family
ID=58337577
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611225997.6A Pending CN106517774A (en) | 2016-12-27 | 2016-12-27 | Preparation method of white-light-emitting glass material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106517774A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793733A (en) * | 2018-06-20 | 2018-11-13 | 昆明理工大学 | A kind of high-melting-point LED fluorescent glass and discharge plasma sintering preparation method |
| CN109320082A (en) * | 2018-09-29 | 2019-02-12 | 江苏锐阳照明电器设备有限公司 | A kind of pyroceram material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103803797A (en) * | 2013-12-25 | 2014-05-21 | 齐鲁工业大学 | Luminescent glass for LED (Light-Emitting Diode) and preparation method of luminescent glass |
| CN104944766A (en) * | 2015-06-08 | 2015-09-30 | 李纯 | Light-emitting glass as well as preparation method and application thereof |
-
2016
- 2016-12-27 CN CN201611225997.6A patent/CN106517774A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103803797A (en) * | 2013-12-25 | 2014-05-21 | 齐鲁工业大学 | Luminescent glass for LED (Light-Emitting Diode) and preparation method of luminescent glass |
| CN104944766A (en) * | 2015-06-08 | 2015-09-30 | 李纯 | Light-emitting glass as well as preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793733A (en) * | 2018-06-20 | 2018-11-13 | 昆明理工大学 | A kind of high-melting-point LED fluorescent glass and discharge plasma sintering preparation method |
| CN109320082A (en) * | 2018-09-29 | 2019-02-12 | 江苏锐阳照明电器设备有限公司 | A kind of pyroceram material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103803797B (en) | A kind of LED fluorescent glass and preparation method thereof | |
| CN104944766B (en) | A kind of fluorescent glass and its preparation method and application | |
| CN106800371B (en) | A kind of high thermal conductivity coefficient borosilicate fluorescent glass material and preparation method thereof | |
| CN104177079B (en) | For Ce:YAG base transparent ceramic containing Sr that white-light LED fluorescence is changed and preparation method thereof | |
| CN101533882A (en) | fluorescent powder prefabricated film for white light LED and preparation method thereof | |
| CN101701683A (en) | Light transmission board pre-fabricated component of white light LED and manufacturing method thereof | |
| CN101656290A (en) | Process for encapsulating light-emitting diode | |
| CN111574062A (en) | Nitride red-light glass and application thereof | |
| CN111153594A (en) | YAG-Ce glass ceramic and preparation method and application thereof | |
| CN101338879A (en) | Method for preparing white light LED utilizing YAG transparent ceramic | |
| CN102709448A (en) | White light LED packaging structure and method | |
| CN103468264A (en) | Manufacture method of polycrystalline Ce:YAG fluorophor | |
| CN106517774A (en) | Preparation method of white-light-emitting glass material | |
| CN107098582B (en) | White light luminescent glass with high thermal stability and borate matrix for LED and preparation method thereof | |
| US9580650B1 (en) | Method of manufacturing Ce:YAG polycrystalline phosphor | |
| CN201237164Y (en) | White light LED | |
| CN109516694B (en) | Fluorescent glass, preparation method thereof and light-emitting device | |
| US20120138854A1 (en) | Green luminescent glass for ultraviolet led and preparation method thereof | |
| CN105347677B (en) | A kind of photic white light glass and its preparation technology | |
| CN101701684A (en) | LED lamp based on blue light and red light chips and manufacturing method thereof | |
| CN114276024B (en) | High-color-rendering composite fluorescent glass and preparation method thereof | |
| CN108793733A (en) | A kind of high-melting-point LED fluorescent glass and discharge plasma sintering preparation method | |
| CN106587601A (en) | Borate red luminescent glass and preparation method thereof | |
| CN101759361A (en) | Rare earth doped luminescent glass and preparation method thereof | |
| Peng et al. | High-power white LED packaging using phosphor-in-glass and its thermal reliability |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| AD01 | Patent right deemed abandoned | ||
| AD01 | Patent right deemed abandoned |
Effective date of abandoning: 20191022 |