CN110256076A - Cr/Ce:YAG fluorescent transparent ceramics and preparation method thereof, preparation system - Google Patents
Cr/Ce:YAG fluorescent transparent ceramics and preparation method thereof, preparation system Download PDFInfo
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Abstract
A kind of Cr/Ce:YAG fluorescent transparent ceramics provided by the invention and preparation method thereof and preparation system use Cr by introducing trivalent chromic ion in Ce:YAG fluorescent transparent ceramics3+It goes to replace Al3+The chemical formula Y of formation3‑xAl5‑yCryO12:Cex, wherein x is 0.001-0.06, y 0-4, controls Ce3+Ion, Cr3+The concentration of ion adjusts Cr3+Ion and Ce3+Energy transfer between ion increases red emission, improves colour rendering index up to 75 or more.
Description
Technical field
The present invention relates to technical field of ceramic material, a kind of Cr/Ce:YAG fluorescent transparent ceramics and its preparation are particularly related to
Method, preparation system.
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.
Currently, white light-emitting diode (wled) as a kind of equipment of artificial light be widely used in room lighting and mostly
Number greenhouse, because of their advantage high energy conversion and long-life.The white-light LED encapsulation mode of the marketization is by Ce:YAG fluorescent powder
It is uniformly mixed with epoxy resin or silica gel, Ce3+Launch yellow light, yellow light and indigo plant after being stimulated by blue light by way of spontaneous radiation
Light combines to generate white light.However the deterioration of polymer (epoxy resin and silica gel), chip and fluorescent powder etc. are encapsulated in WLED
There are some problems in practical application, such as: the degeneration of illumination efficiency, the variation of luminescent color and service life reduction etc., these will
Reduce the comfort level of human eye.Therefore, the appearance of inorganic transparent ceramic material (such as fluorescent transparent ceramics, glass, glass ceramics)
The thermal stability of material can be improved.But YAG fluorescent transparent ceramics cause colour rendering index low, therefore due to lacking RED sector
The supplement of red component is a key of YAG fluorescent transparent ceramic applications, prepares the fluorescent transparent ceramics of high colour developing thus
It is of great significance.
Summary of the invention
In view of the foregoing, it is necessary to provide a kind of improved Cr/Ce:YAG fluorescent transparent ceramics and preparation method thereof and
Preparation system provides the high fluorescent transparent ceramics to develop the color.
Technical solution provided by the invention are as follows: a kind of preparation method of Cr/Ce:YAG fluorescent transparent ceramics, including following step
It is rapid:
By Y2O3、Al2O3、CeO2、Cr2O3Raw material is uniformly mixed after weighing by chemical formula proportion, under the certain pressure time
Mixed powder is pressed into green body；
Green body is further pressed into fine and close biscuit under the certain pressure time；
Biscuit is sintered in vacuum sintering furnace, obtains fluorescence ceramics piece sample；
Gained sample is made annealing treatment, obtaining chemical formula is Y3-xAl5-yCryO12:CexFluorescent transparent ceramics,
Middle x is 0.001-0.06, y 0-4.
Further, pressure is 3-20t in step 1.
Further, the dwell time is 5-20min in step 1.
Further, pressure is 50-300MPa in step 2.
Further, the dwell time is 5-20min in step 2.
Further, sintering condition in step 3: it is warming up to 1400-1800 DEG C with 1-10 DEG C/min, keeps the temperature 2-20h, vacuum
Degree 10-4-10-3Pa。
Further, condition is made annealing treatment in step 4: being warming up to 1200-1600 DEG C with 6-10 DEG C/min, heat preservation 5-10 is small
When.
The present invention separately provides a kind of Cr/Ce:YAG fluorescent transparent ceramics, passes through above-mentioned Cr/Ce:YAG fluorescent transparent ceramics
Preparation method obtain, the fluorescent transparent ceramics have red emission characteristic.
The present invention provides a kind of preparation system of Cr/Ce:YAG fluorescent transparent ceramics again, and the preparation system includes weighing
Equipment, batch mixer, hydraulic press, cold isostatic press, vacuum sintering furnace and high temperature resistance furnace, wherein
Weighing equipment is used for Y2O3、Al2O3、CeO2、Cr2O3Raw material weighing；
Batch mixer, it is uniformly mixed for carrying out various raw materials；
Green body is made for mixed powder to be kept 5-20min duration under 3-20t pressure in hydraulic press；
Fine and close biscuit is made for green body to be kept 5-20min duration under 50-300MPa pressure in cold isostatic press；
Vacuum sintering furnace controls its vacuum degree 10-4-10-3Pa, heating rate is 1-10 DEG C/min, for biscuit to exist
2-20h is kept the temperature at a temperature of 1400-1800 DEG C, sintering obtains fluorescence ceramics piece sample；
High temperature resistance furnace, controlling its heating rate is 6-10 DEG C/min, is used for fluorescence ceramics piece sample in 1200-1600
5-10h is kept the temperature at a temperature of DEG C, it is Y that annealing, which obtains chemical formula,3-xAl5-yCryO12:CexFluorescent transparent ceramics, wherein x is
0.001-0.06, y 0-4.
Further, the chemical formula is Y3-xAl5-yCryO12:CexThe quantum efficiencies of fluorescent transparent ceramics reach
70-85%, colour rendering index are 75 or more.
Compared with prior art, the preparation method of a kind of Cr/Ce:YAG fluorescent transparent ceramics provided by the invention, including with
Lower step: by Y2O3、Al2O3、CeO2、Cr2O3Raw material is uniformly mixed after weighing by chemical formula proportion, will under the certain pressure time
Mixed powder is pressed into green body；Green body is further pressed into fine and close biscuit under the certain pressure time；By biscuit in vacuum
It is sintered in sintering furnace, obtains fluorescence ceramics piece sample；Gained sample is made annealing treatment, obtaining chemical formula is Y3- xAl5-yCryO12:CexFluorescent transparent ceramics, wherein x be 0.001-0.06, y 0-4.The present invention passes through saturating in Ce:YAG fluorescence
Trivalent chromic ion is introduced in bright ceramics, uses Cr3+It goes to replace Al3+The chemical formula Y of formation3-xAl5-yCryO12:Cex, control Ce3+From
Son, Cr3+The concentration of ion adjusts Cr3+Ion and Ce3+Energy transfer between ion increases red emission, improves colour rendering index
Up to 75 or more.
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 difference Cr in an embodiment of the present invention3+The launching light spectrogram of doping fluorescent transparent ceramics.
Fig. 2 is the preparation system schematic diagram of Cr/Ce:YAG fluorescent transparent ceramics in an embodiment of the present invention.
Description of symbols:
| Weighing equipment | 101 |
| Batch mixer | 103 |
| Hydraulic press | 105 |
| Cold isostatic press | 107 |
| Vacuum sintering furnace | 109 |
| High temperature resistance furnace | 111 |
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.
Light source is known as colour rendering to the coloration ability of object, is by reference with same colour temperature or reference light source (incandescent lamp
Or draw light) under object appearance color comparison.As the master that seldom in light source light spectrum or shortage object is reflected under reference light source
When wave, color can be made to generate, and apparent colorshift. color difference degree is bigger, and light source is poorer to the colour rendering of the color.Sunlight
Colour rendering index be defined as 100, the colour rendering index of incandescent lamp is accordingly regarded as ideal reference light source very close to daylight.
Quantum efficiency is an important parameter for describing photoelectric device photoelectric conversion capacity, it is under a certain specific wavelength
The ratio between the average photoelectron number and incident light subnumber for being generated in unit time.
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
Y is pressed using weighing equipment 1012.97Al4.97Cr0.03O12:Ce0.03, stoichiometric ratio weighs Y respectively2O3 6.706g、
Al2O3 5.067g、Cr2O3 0.046g、CeO20.103g is added in ball grinder (i.e. mixing machine 103) with 400r/min revolving speed
It obtains mixture within ball milling 3 hours, then fills this blend into stainless steel mould, use hydraulic press 105 with 10t pressure dry-pressing
10min obtains green body, and it is pressure maintaining in 250MPa cold isostatic press 107 that then green body, which is put into vacuum packaging bag in pressure,
10min obtains biscuit, then biscuit is warming up to 1700 DEG C in vacuum sintering furnace 109 with 3 DEG C/min, keeps the temperature 5 hours, vacuum degree
It is 8 × 10-4, 1500 DEG C then are warming up to 6 DEG C/min in high temperature resistance furnace 111 and is made annealing treatment, and keep the temperature 5 hours, with
Furnace is cooling, and ceramic sheet is finally carried out cutting and polishing processing, and thickness 0.15cm fluorescent transparent ceramics are made, it is saturating to measure the fluorescence
The quantum efficiency of bright ceramics is 81%, colour rendering index 75.
Embodiment 2
Y is pressed using weighing equipment 1012.97Al4.9Cr0.1O12:Ce0.03, stoichiometric ratio weighs Y respectively2O3 6.706g、
Al2O3 4.996g、Cr2O3 0.152g、CeO20.103g is added in ball grinder (i.e. mixing machine 103) with 400r/min revolving speed
It obtains mixture within ball milling 3 hours, then fills this blend into stainless steel mould, use hydraulic press 105 with 10t pressure dry-pressing
10min obtains green body, and it is pressure maintaining in 250MPa cold isostatic press 107 that then green body, which is put into vacuum packaging bag in pressure,
10min obtains biscuit, then biscuit is warming up to 1700 DEG C in vacuum sintering furnace 109 with 3 DEG C/min, keeps the temperature 5 hours, vacuum degree
It is 8 × 10-4, 1500 DEG C then are warming up to 6 DEG C/min in high temperature resistance furnace 111 and is made annealing treatment, and keep the temperature 5 hours, with
Furnace is cooling, and ceramic sheet is finally carried out cutting and polishing processing, and thickness 0.15cm fluorescent transparent ceramics are made, it is saturating to measure the fluorescence
The quantum efficiency of bright ceramics is 78%, colour rendering index 79.
Embodiment 3
Y is pressed using weighing equipment 1012.97Al4.7Cr0.3O12:Ce0.03, stoichiometric ratio weighs Y respectively2O3 6.706g、
Al2O3 4.792g、Cr2O3 0.456g、CeO20.103g is added in ball grinder (i.e. mixing machine 103) with 400r/min revolving speed
It obtains mixture within ball milling 3 hours, then fills this blend into stainless steel mould, use hydraulic press 105 with 10t pressure dry-pressing
10min obtains green body, and it is pressure maintaining in 250MPa cold isostatic press 107 that then green body, which is put into vacuum packaging bag in pressure,
10min obtains biscuit, then biscuit is warming up to 1700 DEG C in vacuum sintering furnace 109 with 3 DEG C/min, keeps the temperature 5 hours, vacuum degree
It is 8 × 10-4, 1500 DEG C then are warming up to 6 DEG C/min in high temperature resistance furnace 111 and is made annealing treatment, and keep the temperature 5 hours, with
Furnace is cooling, and ceramic sheet is finally carried out cutting and polishing processing, and thickness 0.15cm fluorescent transparent ceramics are made, it is saturating to measure the fluorescence
The quantum efficiency of bright ceramics is 74%, colour rendering index 82.
It is as shown in Figure 1 different Cr3+The excitation luminescent spectrum figure of doping fluorescence ceramics built-in testing, as can be seen from Fig.,
Y of the invention3-xAl5-yCryO12:CexFluorescent transparent ceramics there is red emission spectrum in 650-730nm, and with Cr3+
The increase of doping, emissive porwer increase, and red emission spectral red shift, colour rendering index increases；In addition, through measuring Y3-xAl5- yCryO12:CexThe quantum efficiency of fluorescent transparent ceramics reaches 70-85%, colour rendering index 75-85.
Embodiment 4
Y is pressed using weighing equipment 1012.97Al4.7Cr0.3O12:Ce0.03, stoichiometric ratio weighs Y respectively2O3 6.706g、
Al2O3 4.792g、Cr2O3 0.456g、CeO20.103g is added in ball grinder (i.e. mixing machine 103) with 400r/min revolving speed
It obtains mixture within ball milling 3 hours, then fills this blend into stainless steel mould with hydraulic press 105 with 20t pressure dry-pressing 5min
Green body is obtained, it is that pressure maintaining 15min is obtained in 300MPa cold isostatic press 107 that then green body, which is put into vacuum packaging bag in pressure,
Biscuit, then biscuit is warming up to 1800 DEG C in vacuum sintering furnace 109 with 4 DEG C/min, 8 hours are kept the temperature, vacuum degree is 8 × 10-4,
Then 1200 DEG C are warming up to 8 DEG C/min in high temperature resistance furnace 111 to be made annealing treatment, keep the temperature 6 hours, furnace cooling, most
Ceramic sheet is subjected to cutting and polishing processing afterwards, thickness 0.15cm fluorescent transparent ceramics are made, measures fluorescent transparent ceramics
Quantum efficiency is 78%, colour rendering index 83.
Embodiment 5
Y is pressed using weighing equipment 1012.97Al4.97Cr0.03O12:Ce0.03, stoichiometric ratio weighs Y respectively2O3 6.706g、
Al2O3 5.067g、Cr2O3 0.046g、CeO20.103g is added in ball grinder (i.e. mixing machine 103) with 400r/min revolving speed
It obtains mixture within ball milling 3 hours, then fills this blend into stainless steel mould with hydraulic press 105 with 15t pressure dry-pressing 15min
Green body is obtained, it is that pressure maintaining 20min is obtained in 200MPa cold isostatic press 107 that then green body, which is put into vacuum packaging bag in pressure,
Biscuit, then biscuit is warming up to 1550 DEG C in vacuum sintering furnace 109 with 6 DEG C/min, 10 hours are kept the temperature, vacuum degree is 8 × 10-4, 1400 DEG C then are warming up to 8 DEG C/min in high temperature resistance furnace 111 and is made annealing treatment, and keep the temperature 7 hours, furnace cooling,
Ceramic sheet is finally subjected to cutting and polishing processing, thickness 0.15cm fluorescent transparent ceramics are made, measures fluorescent transparent ceramics
Quantum efficiency be 79%, colour rendering index 77.
In other embodiments, the briquetting pressure of green body can be 3-20t, and dwell time 5-20min is not limited to
Above-described embodiment；In other embodiments, the briquetting pressure of biscuit can be 50-300MPa, dwell time 5-20min,
It is not limited to above-described embodiment；In other embodiments, it can control the vacuum degree of vacuum sintering furnace 10-4-10-3Pa range,
Heating rate is 1-10 DEG C/min, and for biscuit to be kept the temperature 2-20h at a temperature of 1400-1800 DEG C, technological parameter is not limited to
Above-described embodiment；In other embodiments, the heating rate that can control high temperature resistance furnace is 6-10 DEG C/min, is used for fluorescence
Potsherd sample keeps the temperature 5-10h at a temperature of 1200-1600 DEG C, is not limited to above-described embodiment.
To sum up, the present invention uses Cr by introducing trivalent chromic ion in Ce:YAG fluorescent transparent ceramics3+It goes to replace Al3+Shape
At chemical formula Y3-xAl5-yCryO12:Cex, wherein x 0.001-0.06, y 0-4 controls Ce3+Ion, Cr3+Ion it is dense
Degree adjusts Cr3+Ion and Ce3+Energy transfer between ion can increase red emission, improve colour rendering index up to 75 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 preparation method of Cr/Ce:YAG fluorescent transparent ceramics, which comprises the following steps:
By Y2O3、Al2O3、CeO2、Cr2O3Raw material is uniformly mixed after weighing by chemical formula proportion, will mixing under the certain pressure time
Powder pressing is at green body；
Green body is further pressed into fine and close biscuit under the certain pressure time；
Biscuit is sintered in vacuum sintering furnace, obtains fluorescence ceramics piece sample；
Gained sample is made annealing treatment, obtaining chemical formula is Y3-xAl5-yCryO12:CexFluorescent transparent ceramics, wherein x is
0.001-0.06, y 0-4.
2. the preparation method of Cr/Ce:YAG fluorescent transparent ceramics according to claim 1, it is characterised in that: pressed in step 1
Power is 3-20t.
3. the preparation method of Cr/Ce:YAG fluorescent transparent ceramics according to claim 1, it is characterised in that: protected in step 1
The pressure time is 5-20min.
4. the preparation method of Cr/Ce:YAG fluorescent transparent ceramics according to claim 1, it is characterised in that: pressed in step 2
Power is 50-300MPa.
5. the preparation method of Cr/Ce:YAG fluorescent transparent ceramics according to claim 1, it is characterised in that: protected in step 2
The pressure time is 5-20min.
6. the preparation method of Cr/Ce:YAG fluorescent transparent ceramics according to claim 1, it is characterised in that: burnt in step 3
Knot condition: it is warming up to 1400-1800 DEG C with 1-10 DEG C/min, keeps the temperature 2-20h, vacuum degree 10-4-10-3Pa。
7. the preparation method of Cr/Ce:YAG fluorescent transparent ceramics according to claim 1, it is characterised in that: moved back in step 4
Fiery treatment conditions: it is warming up to 1200-1600 DEG C with 6-10 DEG C/min, keeps the temperature 5-10 hours.
8. a kind of Cr/Ce:YAG fluorescent transparent ceramics, it is characterised in that: pass through Cr/ such as of any of claims 1-7
The preparation method of Ce:YAG fluorescent transparent ceramics obtains, and the fluorescent transparent ceramics have red emission characteristic.
9. a kind of preparation system of Cr/Ce:YAG fluorescent transparent ceramics, it is characterised in that: the preparation system includes weighing to set
Standby, batch mixer, hydraulic press, cold isostatic press, vacuum sintering furnace and high temperature resistance furnace, wherein
Weighing equipment is used for Y2O3、Al2O3、CeO2、Cr2O3Raw material weighing；
Batch mixer, it is uniformly mixed for carrying out various raw materials；
Green body is made for mixed powder to be kept 5-20min duration under 3-20t pressure in hydraulic press；
Fine and close biscuit is made for green body to be kept 5-20min duration under 50-300MPa pressure in cold isostatic press；
Vacuum sintering furnace controls its vacuum degree 10-4-10-3Pa, heating rate are 1-10 DEG C/min, are used for biscuit in 1400-
2-20h is kept the temperature at a temperature of 1800 DEG C, sintering obtains fluorescence ceramics piece sample；
High temperature resistance furnace, controlling its heating rate is 6-10 DEG C/min, is used for fluorescence ceramics piece sample in 1200-1600 DEG C of temperature
Degree is lower to keep the temperature 5-10h, and it is Y that annealing, which obtains chemical formula,3-xAl5-yCryO12:CexFluorescent transparent ceramics, wherein x is
0.001-0.06, y 0-4.
10. the preparation system of Cr/Ce:YAG fluorescent transparent ceramics according to claim 9, it is characterised in that: the change
Formula is Y3-xAl5-yCryO12:CexThe quantum efficiencies of fluorescent transparent ceramics reach 70-85%, colour rendering index is 75 or more.
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