CN110256072A - Fluorescent transparent ceramics and preparation method thereof - Google Patents
Fluorescent transparent ceramics and preparation method thereof Download PDFInfo
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- CN110256072A CN110256072A CN201910153014.XA CN201910153014A CN110256072A CN 110256072 A CN110256072 A CN 110256072A CN 201910153014 A CN201910153014 A CN 201910153014A CN 110256072 A CN110256072 A CN 110256072A
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Abstract
A kind of fluorescent transparent ceramic preparation provided by the invention, it comprises the steps of: (10%-80%) in mass ratio: (10%-70%): YAG bloom, green powder, the nitride rouge and powder of (10%-80%), it is respectively charged into a cavity of mold, the YAG bloom peak wavelength is 545-580nm, the peak wavelength of the green powder is 520-540nm, and the peak wavelength of the nitride rouge and powder is 615-660nm；S2: the green body of monolith is pressed into using hydraulic press；S3: green body is pressed into fine and close biscuit with cold isostatic press；S4: biscuit is sintered in SPS plasma discharge Fast Sintering furnace, obtains fluorescence ceramics piece sample；S5: resulting fluorescence ceramics piece sample is made annealing treatment in high temperature resistance furnace, obtains fluorescent transparent ceramics.The present invention passes through the mold of colour wheel fluorescence block, three toner bodies are pressed into fine and close biscuit under the certain pressure time, it is sintered out fluorescence ceramics piece using SPS plasma discharge Fast Sintering furnace one-step method, made fluorescence ceramics piece even compact, temperature tolerance are good, quantum efficiency reaches 70-80%.
Description
Technical field
The present invention relates to rare earth luminescent material preparation field more particularly to a kind of fluorescent transparent ceramic preparations.
Background technique
Background that this section is intended to provide an explanation of the embodiments of the present invention set forth in the claims or context.Herein
Description recognizes it is the prior art not because not being included in this section.
The advantages that solid-state lighting (SSL) is due to its environment friendly, luminous efficiency height, service life length, low energy consumption, has developed
As the new lighting source of forth generation.With the continuous development of LED manufacture technology and great power LED, for the application of laser lighting
Demand constantly expands, the stability of dialogue light conversion material and device under conditions of high temperature, long-time, high-power and high brightness
It is required that getting higher.
However under high temperature, high input current density, organic material due to poor heat resistance, it is easy to aging the disadvantages of will lead to light
It declines and phenomena such as color temperature shift, and limits their application.In order to solve these disadvantages, the envelope of more high heat conductance is used in the market
Fill silica gel, glass ceramics, monocrystalline and crystalline ceramics.Latter three is inorganic block materials, itself has higher erosion
Property.
Glass ceramics problem to be solved has: first is that the heat for needing suitable fluorescent powder to be resistant to when glass matrix melting
It corrodes, the ion that in addition glass matrix introduces may have quenching effect, the difference of glass matrix and phosphor indices for shining
The different light transmittance that can reduce glass ceramics.The color rendering index values of common white light LEDs are about in 40-70, and there is also RGB three
Lack red color light component in primary colours and causes the problems such as colour rendering index is low, luminous efficiency is low.
Summary of the invention
In view of the foregoing, it is necessary to which a kind of improved fluorescent transparent ceramics and preparation method thereof are provided.
Technical solution provided by the invention are as follows:
A kind of fluorescent transparent ceramic preparation comprising the steps of:
S1: in mass ratio (10%-80%): (10%-70%): YAG bloom, green powder, the nitride of (10%-80%) are red
Powder is respectively charged into a cavity of mold, and the YAG bloom peak wavelength is 545-580nm, and the peak wavelength of the green powder is
520-540nm, the peak wavelength of the nitride rouge and powder are 615-660nm；
S2: the green body of monolith is pressed into using hydraulic press；
S3: green body is pressed into fine and close biscuit with cold isostatic press；
S4: biscuit is sintered in SPS plasma discharge Fast Sintering furnace, obtains fluorescence ceramics piece sample；
S5: resulting fluorescence ceramics piece sample is made annealing treatment in high temperature resistance furnace, obtains fluorescent transparent ceramics.
Preferably, the green powder is the green powder of LuAG or the green powder of β-sialon.
Preferably, the pressure of hydraulic press is 3-20T, dwell time 5-20min in the S2.
Preferably, cold isostatic press pressure is 50-300MPa, dwell time 5-20min in the S3.
Preferably, it SPS plasma discharge Fast Sintering furnace sintering condition in the S4: is warming up to 100-300 DEG C/min
1400-1600 DEG C, keep the temperature 5-10min, pressure 10-80Mpa.
Preferably, condition is made annealing treatment in the S5: being warming up to 1200-1600 DEG C with 6-10 DEG C/min, heat preservation 1-10 is small
When.
Preferably, the mold is substantially in disk form, and the mold includes bottom plate and surrounds to form cavity with the bottom plate
Side wall, and by the baffle of cavity subregion.
Preferably, the baffle runs through the bottom plate, and the relatively described bottom plate is moved in cavity in telescopic variation, institute
It states and is gradually become smaller at bottom plate described in the width of baffle into cavity.
Preferably, the mould diameter is 20-100mm, and the Sidewall Height is 30-80mm.
Another object of the present invention is that providing a kind of fluorescent transparent ceramics, made by adopting the above technical scheme
It is standby, fluorescent transparent ceramics with a thickness of 0.15-0.20mm, the colour temperature of the fluorescent transparent ceramics is 2800K-6000K, institute
The colour rendering index for stating fluorescent transparent ceramics is 80-90.
Compared with prior art, a kind of fluorescent transparent ceramic preparation provided by the invention comprising the steps of: S1:
In mass ratio (10%-80%): (10%-70%): YAG bloom, green powder, the nitride rouge and powder of (10%-80%) are respectively charged into
One cavity of mold；S2: the green body of monolith is pressed into using hydraulic press；S3: green body is pressed into densification with cold isostatic press
Biscuit；S4: biscuit is sintered in SPS plasma discharge Fast Sintering furnace, obtains fluorescence ceramics piece sample；S5: by institute
The fluorescence ceramics piece sample obtained is made annealing treatment in high temperature resistance furnace, obtains fluorescent transparent ceramics.The present invention passes through colour wheel
Three toner bodies are pressed into fine and close biscuit by the mold of fluorescence block under the certain pressure time, quick using SPS plasma discharge
Sintering furnace one-step method is sintered out fluorescence ceramics piece, and made fluorescence ceramics piece even compact, temperature tolerance are good, quantum efficiency reaches 70-
80%.
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the overall schematic of mold in an embodiment of the present invention.
Description of symbols:
| Mold | 10 |
| Bottom plate | 11 |
| Side wall | 13 |
| Baffle | 15 |
The embodiment of the present invention that the following detailed description will be further explained with reference to the above drawings.
Specific embodiment
In order to be more clearly understood that the above objects, features, and advantages of the embodiment of the present invention, with reference to the accompanying drawing and
The present invention will be described in detail for specific embodiment.It should be noted that in the absence of conflict, the embodiment party of the application
Feature in formula can be combined with each other.
Embodiment in the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, described reality
Applying mode is only some embodiments of the invention, rather than whole embodiments.Based on the embodiment in the present invention, originally
Field those of ordinary skill every other embodiment obtained without making creative work, belongs to this hair
The range of bright embodiment protection.
β-sialon: belonging to one kind of sialon ceramics, and general formula is generally written as Si6-ZAlZOZN8-Z, wherein 0 < Z≤4.2.Its
Crystal grain is usually long column shape, thus the ductile strength of its ceramic body is preferable.
Unless otherwise defined, all technical and scientific terms used herein and the technology for belonging to the embodiment of the present invention
The normally understood meaning of the technical staff in field is identical.Term as used herein in the specification of the present invention is intended merely to
The purpose of specific embodiment is described, it is not intended that in the limitation embodiment of the present invention.
Embodiment 1:
A kind of fluorescent transparent ceramic preparation, it includes following steps:
S1: preparing YAG bloom, green powder, nitride rouge and powder, and in present embodiment, it is 520nm that the green powder, which is peak wavelength,
The green powder of LuAG, the YAG bloom peak wavelength be 545nm, the nitride rouge and powder peak wavelength be 618nm.The YAG is yellow
The ratio of the green powder of powder, LuAG and nitride rouge and powder is 4:2:1, and the quality of total fluorescent powder is 6g.
Referring to Fig. 1, the mold 10 substantially disc, the mold 10 includes being located at bottom in present embodiment
11 periphery of bottom plate 11 and the bottom plate side wall 13, the bottom plate 11, which is directed toward 10 side of mold and is equipped with, is divided into three parts for mold 10
Baffle 15, in present embodiment, the baffle 15 is set as three, and circumferentially array is arranged at the bottom three baffles 15
On plate 11, the baffle 15 is strip, and wherein one end abuts setting on the side wall 13 to three baffles 15, in addition
One end mutually abuts setting.In present embodiment, the baffle 15 is triangle, the gear perpendicular to the section in 11 direction of bottom plate
Wherein a side and the bottom plate 11 are arranged in parallel on plate 15, and in present embodiment, the baffle 15 is along the vertical direction
Scalable setting.In present embodiment, the diameter of the bottom plate 11 is 30mm, and 13 height of side wall is 60mm, the mold
10 materials are stainless steel.In other embodiments, the diameter of the bottom plate 11 can also be arranged between 20-100mm, described
Side wall 13 is highly arranged between 30-80mm, and 15 material of baffle can be set to plastics or rubber.
S2: it is pressed into three color green bodies of monolith using hydraulic press, takes out mold 10 after the completion of compacting.
Three kinds of fluorescent powders are being carried out in pressing process by hydraulic press, the baffle 15 is along the direction perpendicular to bottom plate 11
It is retracted to 11 side of bottom plate, the fluorescent powder positioned at 15 two sides of baffle is contacted with each other, it, can after the completion of compacting
Originally fluorescent powder in separate three is suppressed the three color green bodies to form monolith by realization.
In present embodiment, the pressure of the hydraulic press is 10T, obtains final green body using hydraulic press compacting 10min.
S3: three color green bodies are pressed into fine and close biscuit with cold isostatic press.
In present embodiment, the pressure of the cold isostatic press is 200Mpa, pressing time 5min.
S4: biscuit is sintered in SPS plasma discharge Fast Sintering furnace, obtains fluorescence ceramics piece sample.
In present embodiment, in sintering process, by biscuit in SPS plasma discharge Fast Sintering furnace with 200 DEG C/min liter
Temperature is to 1500 DEG C, wherein the pressure of the SPS plasma discharge Fast Sintering furnace is 60Mpa, soaking time 10min.
S5: resulting fluorescence ceramics piece sample is made annealing treatment in high temperature resistance furnace, obtains fluorescent transparent ceramics.
In present embodiment, the fluorescence ceramics piece sample in high temperature resistance furnace with 6 DEG C/min be warming up to 1200 DEG C into
Row annealing, the furnace cooling after heat preservation 2 hours, obtains ceramic sheet.
Finally, ceramic sheet is carried out cutting and polishing processing, the fluorescence of thickness 0.15mm, colour temperature 6000K, aobvious finger 80 is made
Crystalline ceramics.
Embodiment 2:
The present embodiment is substantially the same manner as Example 1, the difference is that: in present embodiment, the green powder peak value wave
The green powder of β-sialon540 of a length of 540nm, the YAG bloom peak wavelength are 545nm, the nitride rouge and powder peak wavelength
For 630nm.The YAG bloom: the green powder of β-sialon: the ratio of nitride rouge and powder is 4:2:1, total fluorescence described in the present embodiment
The quality of powder is 6g.
Specific steps in present embodiment are as follows: fluorescent powder is fitted into mold 10 formed with 10T pressure dry-pressing 10min it is whole
Three color green bodies of block, then three color green bodies are obtained into biscuit in pressure for pressure maintaining 5min in 250MPa cold isostatic press, biscuit is existed
1450 DEG C, pressure 70MPa are warming up to 300 DEG C/min in SPS sintering furnace, 5min is kept the temperature, is then warming up to 7 DEG C/min
1000 DEG C are made annealing treatment, and keep the temperature 3 hours, furnace cooling.
Ceramic sheet is finally subjected to cutting and polishing processing, the fluorescence of thickness 0.15mm, colour temperature 4500K, aobvious finger 85 is made
Crystalline ceramics.
Embodiment 3:
The present embodiment is essentially identical with Examples 1 and 2, the difference is that: in present embodiment, the green powder is peak
It is worth the green powder of β-sialon that wavelength is 540nm, the YAG bloom peak wavelength is 545nm, the nitride rouge and powder peak wavelength
For 650nm.The YAG bloom: the green powder of β-sialon: the ratio of nitride rouge and powder is 1:2:5, and the quality of total fluorescent powder is 6g.
Specific steps in present embodiment are as follows: fluorescent powder is fitted into mold 10 formed with 10T pressure dry-pressing 10min it is whole
Three color green bodies of block, then three color green bodies are obtained into biscuit in pressure for pressure maintaining 5min in 250MPa cold isostatic press, biscuit is existed
1600 DEG C, pressure 70MPa are warming up to 250 DEG C/min in SPS sintering furnace, 5min is kept the temperature, is then warming up to 6 DEG C/min
1000 DEG C are made annealing treatment, and keep the temperature 2 hours, furnace cooling.
Ceramic sheet is finally subjected to cutting and polishing processing, the fluorescence of thickness 0.20mm, colour temperature 2800K, aobvious finger 90 is made
Crystalline ceramics.
Embodiment 4:
The present embodiment and embodiment 1-3 are essentially identical, the difference is that: in present embodiment, the green powder is peak
It is worth the green powder of LuAG that wavelength is 535nm, the YAG bloom peak wavelength is 580nm, and the nitride rouge and powder peak wavelength is
650nm.The YAG bloom: the green powder of LuAG: the ratio of nitride rouge and powder is 3:1:5, and the quality of total fluorescent powder is 6g.
Specific steps in present embodiment are as follows: fluorescent powder is fitted into mold 10 formed with 10T pressure dry-pressing 10min it is whole
Three color green bodies of block, then three color green bodies are obtained into biscuit in pressure for pressure maintaining 5min in 200MPa cold isostatic press, biscuit is existed
1500 DEG C, pressure 60MPa are warming up to 300 DEG C/min in SPS sintering furnace, 10min is kept the temperature, is then warming up to 8 DEG C/min
1000 DEG C are made annealing treatment, and keep the temperature 1 hour, furnace cooling.
Ceramic sheet is finally subjected to cutting and polishing processing, the fluorescence of thickness 0.15mm, colour temperature 3000K, aobvious finger 90 is made
Crystalline ceramics.
The present invention passes through the mold of colour wheel fluorescence block, and three toner bodies are pressed into fine and close element under the certain pressure time
Base is sintered out fluorescence ceramics piece using SPS plasma discharge Fast Sintering furnace one-step method, and made fluorescent transparent ceramics uniformly cause
It is close, temperature tolerance is good, quantum efficiency reaches 70-80%, and colour rendering index reaches 80 or more.
Embodiment of above is only to illustrate the technical solution of the embodiment of the present invention rather than limits, although referring to above preferable
The embodiment of the present invention is described in detail in embodiment, those skilled in the art should understand that, it can be to this hair
The technical solution of bright embodiment is modified or equivalent replacement should not all be detached from the embodiment of the present invention technical solution spirit and
Range.
Claims (10)
1. a kind of fluorescent transparent ceramic preparation, it is characterised in that: comprise the steps of:
S1: in mass ratio (10%-80%): (10%-70%): YAG bloom, green powder, the nitride rouge and powder of (10%-80%),
It is respectively charged into a cavity of mold, the YAG bloom peak wavelength is 545-580nm, and the peak wavelength of the green powder is 520-
540nm, the peak wavelength of the nitride rouge and powder are 615-660nm；
S2: the green body of monolith is pressed into using hydraulic press；
S3: green body is pressed into fine and close biscuit with cold isostatic press；
S4: biscuit is sintered in SPS plasma discharge Fast Sintering furnace, obtains fluorescence ceramics piece sample；
S5: resulting fluorescence ceramics piece sample is made annealing treatment in high temperature resistance furnace, obtains fluorescent transparent ceramics.
2. the fluorescent transparent ceramic preparation of three colors according to claim 1, it is characterised in that: the green powder be the green powder of LuAG or
The green powder of β-sialon.
3. the fluorescent transparent ceramic preparation of three colors according to claim 1, it is characterised in that: the pressure of hydraulic press in the S2
For 3-20T, dwell time 5-20min.
4. the fluorescent transparent ceramic preparation of three colors according to claim 1, it is characterised in that: cold isostatic press pressure in the S3
Power is 50-300MPa, dwell time 5-20min.
5. the fluorescent transparent ceramic preparation of three colors according to claim 1, it is characterised in that: SPS plasma is put in the S4
Electric Fast Sintering furnace sintering condition: it is warming up to 1400-1600 DEG C with 100-300 DEG C/min, keeps the temperature 5-10min, pressure 10-
80Mpa。
6. the fluorescent transparent ceramic preparation of three colors according to claim 1, it is characterised in that: make annealing treatment item in the S5
Part: it is warming up to 1200-1600 DEG C with 6-10 DEG C/min, keeps the temperature 1-10 hours.
7. the fluorescent transparent ceramic preparation of three colors according to claim 1, it is characterised in that: the mold is substantially in disk
Shape, the mold include bottom plate and surround the side wall to form cavity with the bottom plate, and by the baffle of cavity subregion.
8. according to the fluorescent transparent ceramic preparation of three color of claim 7, it is characterised in that: the baffle runs through the bottom
Plate, and the relatively described bottom plate is moved in cavity in telescopic variation, at bottom plate described in the width of the baffle into cavity by
Gradual change is small.
9. according to the fluorescent transparent ceramic preparation of three color of claim 7, it is characterised in that: the mould diameter is 20-
100mm, the Sidewall Height are 30-80mm.
10. a kind of fluorescent transparent ceramics, it is characterised in that: standby using any fluorescent transparent ceramic system of claim 1-9
It is prepared by method, fluorescent transparent ceramics with a thickness of 0.15-0.20mm, the colour temperature of the fluorescent transparent ceramics is
2800K-6000K, the colour rendering index of the fluorescent transparent ceramics are 80-90.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112341183A (en) * | 2020-11-09 | 2021-02-09 | 新沂市锡沂高新材料产业技术研究院有限公司 | Preparation method of laser-illuminated fluorescent composite ceramic optical fiber |
| CN113402269A (en) * | 2021-06-29 | 2021-09-17 | 南通大学 | Preparation method of three-color transparent fluorescent ceramic capable of adjusting white light of different degrees |
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| CN113402269A (en) * | 2021-06-29 | 2021-09-17 | 南通大学 | Preparation method of three-color transparent fluorescent ceramic capable of adjusting white light of different degrees |
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