CN102620167B - Transparent ceramic white light emitting diode (LED) and preparation method thereof - Google Patents
Transparent ceramic white light emitting diode (LED) and preparation method thereof Download PDFInfo
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- CN102620167B CN102620167B CN201210065895.8A CN201210065895A CN102620167B CN 102620167 B CN102620167 B CN 102620167B CN 201210065895 A CN201210065895 A CN 201210065895A CN 102620167 B CN102620167 B CN 102620167B
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Abstract
The invention provides a transparent ceramic white light emitting diode (LED), which comprises a bracket, a blue LED chip and cerium-doped yttrium aluminum garnet transparent ceramic wafer, wherein the chemical formula of a material of the cerium-doped yttrium aluminum garnet transparent ceramic wafer is (Y1.xCex) 3Al5O12; and in the formula, x is greater than or equal to 0.0005 but less than or equal to 0.005. A packaging method of the transparent ceramic white LED comprises the following steps that: (1) the blue LED chip is put into a groove arranged in the bracket; (2) a gold wire of the blue LED chip is welded with an electrode mounted at the bottom of the bracket; (3) silica gel is filled into the groove of the bracket, and the cerium-doped yttrium aluminum garnet transparent ceramic wafer is covered on the silica gel so as to combine the members; and (4) a combined body formed in the step (3) is baked at a temperature of 100 DEG C to 120 DEG C until the silica gel is cured, and after the silica gel is cured and the cerium-doped yttrium aluminum garnet transparent ceramic wafer and the blue LED chip are fixedly arranged on the bracket, the transparent ceramic white LED is formed.
Description
Technical field
The present invention relates to white light LEDs field, particularly a kind of crystalline ceramics white light LEDs and preparation method thereof.
Background technology
The semiconductor lighting that the light emitting diode (LED) of take is master is the high-technology field that 21 century has development prospect most.Semiconductor light sources as a kind of novelty, the remarkable advantages such as white light LEDs is high with its efficiency, power consumption is little, the life-span is long, solid-state energy-conservation and environmental protection, really lighted " radiance of green illumination ", this is that many traditional light sources are incomparable, thereby is with a wide range of applications.Its application comprises liquid crystal display (LCD) backlight (automobile, soniscope dash board, mobile phone backlight plate), traffic lights, room lighting, plaza lighting etc.The demand that is subject to the field high speed developments such as mobile phone, automobile industry and general lighting market, people sharply increase the demand of white light LEDs.Therefore, the market potential of white light LEDs can be described as quite huge.
The mainstream technology of white light LEDs is still fluorescent material conversion at present, is about to fluorescent material Y
3al
5o
12: Ce (YAG:Ce) mixes with casting glue, is then coated on blue-light LED chip, is changed and is formed white light, the about 2mm of fluorescent coating thickness, the conventional Merlon (PC) of protection lens or the lucite of outside by wavelength.Due to the structure of existing white light LEDs and the performance of fluorescent material, make existing white light LEDs mainly deposit following problem:
1, light extraction efficiency is not high.Conventional fluorescent material particle diameter is more than 1um, and refractive index is more than or equal to 1.85, and embedding silica gel refractive index is generally in 1.5 left and right, because refractive index between the two is not mated, and fluorescent material particle diameter is much larger than the light scattering limit, thereby there is light scattering on fluorescent powder grain surface, reduced light extraction efficiency.
2, poor heat resistance.Along with temperature rises, fluorescent material quantum efficiency reduces, and bright dipping reduces, and radiation wavelength also can change, thereby causes the variation of white light LED color temperature, colourity, and higher temperature also can be accelerated the aging of fluorescent material.Reason is that fluorescent coating is to be formed by epoxy or silica gel and fluorescent material allotment, and heat dispersion is poor, and when being subject to the radiation of purple light or ultraviolet light, easily occurrence temperature quencher and aging, reduces luminous efficiency.
3, heat dispersion is not good.The multiplex PC of lens case of conventional white light LEDs, its temperature can not surpass 110 ℃, and thermal conductivity is not high, be 0.1975W/mK, so heat dispersion is not good.The solution of these problems is keys of LED fast development.
In order to address the above problem, have many patents or patent application to come out:
CN1815765A discloses a kind of YAG chip-type white-light light-emitting-diode and method for packing thereof, and rear-earth-doped YAG wafer is used as to fluorescent material to substitute fluorescent material.But due to the restriction of crystal growth aspect, large-sized YAG monocrystal material needs special equipment and complicated technique, with ceramic phase ratio, its manufacturing cycle is long, cost is higher, be easy to cracking, therefore the application of the method is restricted.
CN101697367A discloses a kind of method of utilizing crystalline ceramics to prepare LED, and the method joins quantitative fluorescent material in transparent ceramic powder, after fully mixing, by ceramic preparation technology, prepares fluorescence crystalline ceramics.Described fluorescent material comprises that one or more in yellow, redness, green, orange, blue, purple fluorescence powder mix in proportion, and the material of described transparent ceramic powder is a kind of in magnesium aluminate spinel, yttrium-aluminium-garnet, yittrium oxide, aluminum oxynitride etc.The problem of this kind of method existence is: fluorescent material does not mate with ceramic powder lattice paprmeter, refractive index etc., thereby can not dissolve each other completely in sintering process, prepared crystalline ceramics uniformity, light transmittance are not high, cause the emergent light of white LED lamp of encapsulation inhomogeneous in spatial distribution, light extraction efficiency is not high.
CN201576698U discloses a kind of transparent ceramic white light LED device, comprise the block crystalline ceramics illuminator as luminescent material, the carrier of LED chip and carrying LED chip and crystalline ceramics illuminator, LED chip is positioned at the bottom portion of groove that carrier is offered, and crystalline ceramics illuminator directly overlays on LED chip or is embedded in carrier.Although replacing fluorescent material with block crystalline ceramics illuminator, this patent effectively reduced scattering of light, be conducive to improve luminous efficiency, preparation with respect to monocrystal material, technique is more simplified, but the composition of this patent unexposed described block crystalline ceramics illuminator, also the luminous efficiency of unexposed its transparent ceramic white light LED device, and the composition of crystalline ceramics illuminator is one of key factor to the raising of luminous efficiency.In addition, its LED chip is positioned at the bottom portion of groove that carrier is offered, crystalline ceramics illuminator directly overlays on LED chip can not realize their fixing on carrier, to the normal operation of transparent ceramic white light LED device and service life, also can impact, LED chip inlaying on carrier can make the preparation section of carrier increase.
Summary of the invention
The object of this invention is to provide a kind of crystalline ceramics white light LEDs and preparation method thereof, further to improve the luminous efficiency of white light LEDs, improve radiating condition, make its working stability, long service life, encapsulate simpler.
Crystalline ceramics white light LEDs of the present invention, comprise support, blue-light LED chip and crystalline ceramics fluorophor, described crystalline ceramics fluorophor is cerium dopping yttrium aluminum garnet transparent ceramic sheet, blue-light LED chip is positioned at the set groove of support and is connected with the electrode of frame bottom installation, cerium dopping yttrium aluminum garnet transparent ceramic sheet covers blue-light LED chip, by the silica gel being filled between cerium dopping yttrium aluminum garnet transparent ceramic sheet and blue-light LED chip, described sheet of transparent ceramic and described LED chip is fixed on support.
Crystalline ceramics white light LEDs of the present invention, its cerium dopping yttrium aluminum garnet transparent ceramic sheet chemical formula is (Y
1-xce
x)
3al
5o
12material make, 0.0005≤x≤0.005 in formula.
Crystalline ceramics white light LEDs of the present invention, the thickness of its cerium dopping yttrium aluminum garnet transparent ceramic sheet is 0.1mm～1.0mm.
The preparation method of above-mentioned cerium dopping yttrium aluminum garnet transparent ceramic sheet is: according to chemical formula (Y
1-xce
x)
3al
5o
12(0.0005≤x≤0.005) metering yttrium salt, aluminium salt and cerium salt, with deionized water dissolving and mix, be mixed with Al by yttrium salt, aluminium salt and cerium salt
3+concentration is the mixing salt solution of 0.1mol/L～0.2mol/L; By NH
4hCO
3be dissolved in alcohol-water double solvents preparation NH
4hCO
3concentration is the precipitant solution of 0.5mol/L～2mol/L, and the volume ratio of described ethanol and water is 0.5: 1～1.2: 1; Described mixing salt solution is titrated in described precipitant solution at normal pressure, 10 ℃～20 ℃, and titration finishes rear ageing at least 10 hours, then, through vacuum filtration, washing, oven dry, obtains presoma; Described presoma, 1100～1250 ℃ of roastings 2～3 hours, is obtained to cerium doped yttrium aluminum garnet powder; Described cerium doped yttrium aluminum garnet powder is formed to biscuit through dry-pressing formed and isostatic cool pressing, then biscuit is put in vacuum sintering furnace 1700～1780 ℃ of sintering at least 10 hours, obtain cerium dopping yttrium aluminum garnet transparent ceramic sheet.
In the preparation method of above-mentioned cerium dopping yttrium aluminum garnet transparent ceramic sheet, described yttrium salt is Y (NO
3)
3or YCl
3, described aluminium salt is NH
4al (SO
4)
2or Al (NO
3)
3, described cerium salt is Ce (NO
3)
3.
The present invention has following beneficial effect:
(1) illuminator due to crystalline ceramics white light LEDs of the present invention is to be (Y with chemical formula
1-xce
x)
3al
5o
12the sheet of transparent ceramic that the material of (0.0005≤x≤0.005) is made, the refractive index of described sheet of transparent ceramic is 1.85 (400nm places), thereby can improve the luminescent properties of white light LED part, make its light extraction efficiency high (light efficiency can reach 99.48lm/W, sees embodiment 2).
(2) in the illuminator of crystalline ceramics white light LEDs of the present invention, the thermal conductivity of its cerium dopping yttrium aluminum garnet transparent ceramic sheet is 12.9W/mK, 5～40 times of silica gel thermal conductivity, be epoxy resin and Merlon (PC) thermal conductivity 65 times (thermal conductivity of epoxy resin is 0.19W/mK, the thermal conductivity of silica gel is 0.3～2.5W/mK, the thermal conductivity of Merlon (PC) lens case is 0.1975W/mK), thereby can effectively improve the radiating effect of blue-light LED chip, improve the stability of white light LEDs.
(3) crystalline ceramics white light LEDs of the present invention, its illuminator cerium dopping yttrium aluminum garnet transparent ceramic sheet is high temperature resistant, heat endurance is high, mechanical property good, transparency is high, thereby without adding again lens case, make that device is more wear-resistant, shock resistance, can apply in hot environment.
(4) because cerium dopping yttrium aluminum garnet transparent ceramic sheet can accurately be controlled on size and shape, thereby can simplify integrated Packaging Technology, improve and make effect.
Accompanying drawing explanation
Fig. 1 is the structural representation of crystalline ceramics white light LEDs of the present invention;
Fig. 2 is the top view of Fig. 1, is the state of removing cerium dopping yttrium aluminum garnet transparent ceramic sheet and silica gel in figure;
Fig. 3 is the spectral power distribution figure of crystalline ceramics white light LEDs described in embodiment 1;
Fig. 4 is the spectral power distribution figure of crystalline ceramics white light LEDs described in embodiment 2;
Fig. 5 is the spectral power distribution figure of crystalline ceramics white light LEDs described in embodiment 3.
In figure, 1-support, 2-blue-light LED chip, 3-cerium dopping yttrium aluminum garnet transparent ceramic sheet, 4-silica gel, 5-gold thread, 6-electrode.
The specific embodiment
Below by embodiment, crystalline ceramics white light LEDs of the present invention and preparation method thereof is described further.In following embodiment, the model of blue-light LED chip is wafer chip ES-CADBV45H, purchased from Shenzhen Shun Bai Science and Technology Ltd.; Polyamide for support (PPA) and copper product preparation, silica gel is transparent silica gel.
In the present embodiment, the structure of crystalline ceramics white light LEDs as shown in Figure 1 and Figure 2, comprise support 1, blue-light LED chip 2 and cerium dopping yttrium aluminum garnet transparent ceramic sheet 3, support is for arranging reeded Rotary-table, cerium dopping yttrium aluminum garnet transparent ceramic sheet 3 is the disk of thickness 1mm, with chemical formula, is (Y
0.995ce
0.005)
3al
5o
12material make, preparation method is as follows: according to the composition metering Y (NO in above-mentioned chemical formula
3)
3, NH
4al (SO
4)
2, Ce (NO
3)
3, by Y (NO
3)
3, NH
4al (SO
4)
2, Ce (NO
3)
3with deionized water dissolving and mix, be mixed with Al
3+concentration is the mixing salt solution of 0.1mol/L.By NH
4hCO
3be dissolved in alcohol-water double solvents preparation NH
4hCO
3concentration is the precipitant solution of 1mol/L, and the volume ratio of described ethanol and water is 0.5: 1; Described mixing salt solution is titrated in described precipitant solution at normal pressure, 15 ℃, and titration finishes rear ageing 10 hours; The precipitation solution good to ageing carries out vacuum filtration, obtains milky white precipitate thing, then by deionized water by sediment undergoes washing 3 times, remove foreign ion, then clean 2 times with absolute ethyl alcohol, remove moisture; White depositions after washing is put into drying box, at normal pressure, 90 ℃ of dry presomas that obtain for 24 hours; Presoma, 1100 ℃ of roastings 3 hours, is obtained to cerium doped yttrium aluminum garnet powder.Described cerium doped yttrium aluminum garnet powder is formed to the circular biscuit that thickness is 1mm through dry-pressing formed and isostatic cool pressing, more described biscuit is put in vacuum sintering furnace 1730 ℃ of sintering 10 hours, obtain cerium dopping yttrium aluminum garnet transparent ceramic sheet.
Blue-light LED chip 2 is placed in the set groove of support 1, by the gold thread of blue-light LED chip 25 and electrode 6 welding that are arranged on frame bottom, then silica gel 4 is filled in the groove of support, the about 0.6mm of filling thickness, again cerium dopping yttrium aluminum garnet transparent ceramic sheet 3 is covered to the combination that completes each member on silica gel 4, continue after by form assembly put into baking oven, at 120 ℃, be baked to silica gel and solidify (approximately 4 hours), after silica gel solidifies, described cerium doped yttrium aluminum garnet potsherd and blue-light LED chip are fixed on support, form Fig. 1, crystalline ceramics white light LEDs shown in Fig. 2.
The prepared crystalline ceramics white light LEDs of the present embodiment is under 350mA constant current drives, and its spectral power distribution figure as shown in Figure 3.Its performance indications are as follows:
Light efficiency: 96.86lm/W
Colour rendering index: 56.8
Colour temperature: 4252K.
In the present embodiment, the structure of crystalline ceramics white light LEDs as shown in Figure 1 and Figure 2, comprise support 1, blue-light LED chip 2 and cerium dopping yttrium aluminum garnet transparent ceramic sheet 3, support is for arranging reeded Rotary-table, cerium dopping yttrium aluminum garnet transparent ceramic sheet 3 is the disk of thickness 1mm, with chemical formula, is (Y
0.999ce
0.001)
3al
5o
12material make, preparation method is as follows: according to the composition metering Y (NO in above-mentioned chemical formula
3)
3, NH
4al (SO
4)
2, Ce (NO
3)
3, by Y (NO
3)
3, NH
4al (SO
4)
2, Ce (NO
3)
3with deionized water dissolving and mix, be mixed with Al
3+concentration is the mixing salt solution of 0.15mol/L.By NH
4hCO
3be dissolved in alcohol-water double solvents preparation NH
4hCO
3concentration is the precipitant solution of 0.5mol/L, and the volume ratio of described ethanol and water is 1: 1; Described mixing salt solution is titrated in described precipitant solution at normal pressure, 20 ℃, and titration finishes rear ageing 12 hours; The precipitation solution good to ageing carries out vacuum filtration, obtains milky white precipitate thing, then by deionized water by sediment undergoes washing 3 times, remove foreign ion, then clean 2 times with absolute ethyl alcohol, remove moisture; White depositions after washing is put into drying box, at normal pressure, 90 ℃ of dry presomas that obtain for 24 hours; Presoma, 1250 ℃ of roastings 2 hours, is obtained to cerium doped yttrium aluminum garnet powder.Described cerium doped yttrium aluminum garnet powder is formed to the circular biscuit that thickness is 1mm through dry-pressing formed and isostatic cool pressing, more described biscuit is put in vacuum sintering furnace 1750 ℃ of sintering 12 hours, obtain cerium dopping yttrium aluminum garnet transparent ceramic sheet.
In the present embodiment, combination and the method for packing of each member of crystalline ceramics white light LEDs or device are identical with embodiment 1.
The prepared crystalline ceramics white light LEDs of the present embodiment is under 350mA constant current drives, and its spectral power distribution figure as shown in Figure 4.Its performance indications are as follows:
Light efficiency: 99.48lm/W
Colour rendering index: 60.3
Colour temperature: 4804K.
Embodiment 3
In the present embodiment, the structure of crystalline ceramics white light LEDs as shown in Figure 1 and Figure 2, comprise support 1, blue-light LED chip 2 and cerium dopping yttrium aluminum garnet transparent ceramic sheet 3, support is for arranging reeded Rotary-table, cerium dopping yttrium aluminum garnet transparent ceramic sheet 3 is the disk of thickness 1mm, with chemical formula, is (Y
0.9995ce
0.0005)
3al
5o
12material make, preparation method is as follows: according to the composition metering Y (NO in above-mentioned chemical formula
3)
3, Al (NO
3)
3, Ce (NO
3)
3, by Y (NO
3)
3, Al (NO
3)
3, Ce (NO
3)
3with deionized water dissolving and mix, be mixed with Al
3+concentration is the mixing salt solution of 0.2mol/L.By NH
4hCO
3be dissolved in alcohol-water double solvents preparation NH
4hCO
3concentration is the precipitant solution of 2mol/L, and the volume ratio of described ethanol and water is 1.2: 1; Described mixing salt solution is titrated in described precipitant solution at normal pressure, 10 ℃, and titration finishes rear ageing 10 hours; The precipitation solution good to ageing carries out vacuum filtration, obtains milky white precipitate thing, then by deionized water by sediment undergoes washing 3 times, remove foreign ion, then clean 2 times with absolute ethyl alcohol, remove moisture; White depositions after washing is put into drying box, at normal pressure, 90 ℃ of dry presomas that obtain for 24 hours; Presoma, 1200 ℃ of roastings 2.5 hours, is obtained to cerium doped yttrium aluminum garnet powder.Described cerium doped yttrium aluminum garnet powder is formed to the circular biscuit that thickness is 1mm through dry-pressing formed and isostatic cool pressing, more described biscuit is put in vacuum sintering furnace 1780 ℃ of sintering 10 hours, obtain cerium dopping yttrium aluminum garnet transparent ceramic sheet.
In the present embodiment, combination and the method for packing of each member of crystalline ceramics white light LEDs or device are identical with embodiment 1.
The prepared crystalline ceramics white light LEDs of the present embodiment is under 350mA constant current drives, and its spectral power distribution figure as shown in Figure 5.Its performance indications are as follows:
Light efficiency: 85.11lm/W
Colour rendering index: 67.4
Colour temperature: 6560K.
Embodiment 4
In the present embodiment, the structure of crystalline ceramics white light LEDs as shown in Figure 1 and Figure 2, comprise support 1, blue-light LED chip 2 and cerium dopping yttrium aluminum garnet transparent ceramic sheet 3, support is for arranging reeded Rotary-table, cerium dopping yttrium aluminum garnet transparent ceramic sheet 3 is the disk of thickness 0.1mm, with chemical formula, is (Y
0.995ce
0.005)
3al
5o
12material make, preparation method is as follows: according to the composition metering YCl in above-mentioned chemical formula
3, Al (NO
3)
3, Ce (NO
3)
3, by YCl
3, Al (NO
3)
3, Ce (NO
3)
3with deionized water dissolving and mix, be mixed with Al
3+concentration is the mixing salt solution of 0.15mol/L.By NH
4hCO
3be dissolved in alcohol-water double solvents preparation NH
4hCO
3concentration is the precipitant solution of 1mol/L, and the volume ratio of described ethanol and water is 0.5: 1; Described mixing salt solution is titrated in described precipitant solution at normal pressure, 15 ℃, and titration finishes rear ageing 10 hours; The precipitation solution good to ageing carries out vacuum filtration, obtains milky white precipitate thing, then by deionized water by sediment undergoes washing 3 times, remove foreign ion, then clean 2 times with absolute ethyl alcohol, remove moisture; White depositions after washing is put into drying box, at normal pressure, 90 ℃ of dry presomas that obtain for 24 hours; Presoma, 1100 ℃ of roastings 3 hours, is obtained to cerium doped yttrium aluminum garnet powder.Described cerium doped yttrium aluminum garnet powder is formed to the circular biscuit that thickness is 0.1mm through dry-pressing formed and isostatic cool pressing, more described biscuit is put in vacuum sintering furnace 1750 ℃ of sintering 10 hours, obtain cerium dopping yttrium aluminum garnet transparent ceramic sheet.
Blue-light LED chip 2 is placed in the set groove of support 1, by the gold thread of blue-light LED chip 25 and electrode 6 welding that are arranged on frame bottom, then silica gel 4 is filled in the groove of support, the about 0.3mm of filling thickness, again cerium dopping yttrium aluminum garnet transparent ceramic sheet 3 is covered to the combination that completes each member on silica gel 4, continue after by form assembly put into baking oven, at 100 ℃, be baked to silica gel and solidify (approximately 3.5 hours), after silica gel solidifies, described cerium doped yttrium aluminum garnet potsherd and blue-light LED chip are fixed on support, form Fig. 1, crystalline ceramics white light LEDs shown in Fig. 2.
The prepared crystalline ceramics white light LEDs of the present embodiment is under 350mA constant current drives, and its spectral power distribution figure as shown in Figure 3.Its performance indications are as follows:
Light efficiency: 55.92lm/W
Colour rendering index: 73.4
Colour temperature: 8640K.
In the present embodiment, the structure of crystalline ceramics white light LEDs as shown in Figure 1 and Figure 2, comprise support 1, blue-light LED chip 2 and cerium dopping yttrium aluminum garnet transparent ceramic sheet 3, support is for arranging reeded Rotary-table, cerium dopping yttrium aluminum garnet transparent ceramic sheet 3 is the disk of thickness 0.4mm, with chemical formula, is (Y
0.999ce
0.001)
3al
5o
12material make, preparation method is as follows: according to the composition metering YCl in above-mentioned chemical formula
3, Al (NO
3)
3, Ce (NO
3)
3, by YCl
3, Al (NO
3)
3, Ce (NO
3)
3with deionized water dissolving and mix, be mixed with Al
3+concentration is the mixing salt solution of 0.1mol/L.By NH
4hCO
3be dissolved in alcohol-water double solvents preparation NH
4hCO
3concentration is the precipitant solution of 0.5mol/L, and the volume ratio of described ethanol and water is 1: 1; Described mixing salt solution is titrated in described precipitant solution at normal pressure, 20 ℃, and titration finishes rear ageing 11 hours; The precipitation solution good to ageing carries out vacuum filtration, obtains milky white precipitate thing, then by deionized water by sediment undergoes washing 3 times, remove foreign ion, then clean 2 times with absolute ethyl alcohol, remove moisture; White depositions after washing is put into drying box, at normal pressure, 90 ℃ of dry presomas that obtain for 24 hours; Presoma, 1250 ℃ of roastings 2 hours, is obtained to cerium doped yttrium aluminum garnet powder.Described cerium doped yttrium aluminum garnet powder is formed to the circular biscuit that thickness is 0.4mm through dry-pressing formed and isostatic cool pressing, more described biscuit is put in vacuum sintering furnace 1700 ℃ of sintering 12 hours, obtain cerium dopping yttrium aluminum garnet transparent ceramic sheet.
Blue-light LED chip 2 is placed in the set groove of support 1, by the gold thread of blue-light LED chip 25 and electrode 6 welding that are arranged on frame bottom, then silica gel 4 is filled in the groove of support, the about 0.4mm of filling thickness, again cerium dopping yttrium aluminum garnet transparent ceramic sheet 3 is covered to the combination that completes each member on silica gel 4, continue after by form assembly put into baking oven, at 110 ℃, be baked to silica gel and solidify (approximately 3.5 hours), after silica gel solidifies, described cerium doped yttrium aluminum garnet potsherd and blue-light LED chip are fixed on support, form Fig. 1, crystalline ceramics white light LEDs shown in Fig. 2.
The prepared crystalline ceramics white light LEDs of the present embodiment is under 350mA constant current drives, and its spectral power distribution figure as shown in Figure 4.Its performance indications are as follows:
Light efficiency: 47.1lm/W
Colour rendering index: 73.8
Colour temperature: 8316K.
In the present embodiment, the structure of crystalline ceramics white light LEDs as shown in Figure 1 and Figure 2, comprise support 1, blue-light LED chip 2 and cerium dopping yttrium aluminum garnet transparent ceramic sheet 3, support is for arranging reeded Rotary-table, cerium dopping yttrium aluminum garnet transparent ceramic sheet 3 is the disk of thickness 0.7mm, with chemical formula, is (Y
0.9995ce
0.0005)
3al
5o
12material make, preparation method is as follows: according to the composition metering YCl in above-mentioned chemical formula
3, Al (NO
3)
3, Ce (NO
3)
3, by YCl
3, Al (NO
3)
3, Ce (NO
3)
3with deionized water dissolving and mix, be mixed with Al
3+concentration is the mixing salt solution of 0.2mol/L.By NH
4hCO
3be dissolved in alcohol-water double solvents preparation NH
4hCO
3concentration is the precipitant solution of 2mol/L, and the volume ratio of described ethanol and water is 1.2: 1; Described mixing salt solution is titrated in described precipitant solution at normal pressure, 10 ℃, and titration finishes rear ageing 10 hours; The precipitation solution good to ageing carries out vacuum filtration, obtains milky white precipitate thing, then by deionized water by sediment undergoes washing 3 times, remove foreign ion, then clean 2 times with absolute ethyl alcohol, remove moisture; White depositions after washing is put into drying box, at normal pressure, 90 ℃ of dry presomas that obtain for 24 hours; Presoma, 1200 ℃ of roastings 2.5 hours, is obtained to cerium doped yttrium aluminum garnet powder.Described cerium doped yttrium aluminum garnet powder is formed to the circular biscuit that thickness is 0.7mm through dry-pressing formed and isostatic cool pressing, more described biscuit is put in vacuum sintering furnace 1780 ℃ of sintering 10 hours, obtain cerium dopping yttrium aluminum garnet transparent ceramic sheet.
Blue-light LED chip 2 is placed in the set groove of support 1, by the gold thread of blue-light LED chip 25 and electrode 6 welding that are arranged on frame bottom, then silica gel 4 is filled in the groove of support, the about 0.5mm of filling thickness, again cerium dopping yttrium aluminum garnet transparent ceramic sheet 3 is covered to the combination that completes each member on silica gel 4, continue after by form assembly put into baking oven, at 120 ℃, be baked to silica gel and solidify (approximately 4 hours), after silica gel solidifies, described cerium doped yttrium aluminum garnet potsherd and blue-light LED chip are fixed on support, form Fig. 1, crystalline ceramics white light LEDs shown in Fig. 2.
The prepared crystalline ceramics white light LEDs of the present embodiment is under 350mA constant current drives, and its spectral power distribution figure as shown in Figure 5.Its performance indications are as follows:
Light efficiency: 59.85lm/W
Colour rendering index: 76.4
Colour temperature: 10084K.
Claims (4)
1. a crystalline ceramics white light LEDs, comprise support (1), blue-light LED chip (2) and crystalline ceramics fluorophor, it is characterized in that described crystalline ceramics fluorophor is cerium dopping yttrium aluminum garnet transparent ceramic sheet (3), blue-light LED chip (2) is positioned at the set groove of support (1) and is connected with the electrode (6) of frame bottom installation, cerium dopping yttrium aluminum garnet transparent ceramic sheet (3) covers blue-light LED chip (2), by the silica gel (4) being filled between cerium dopping yttrium aluminum garnet transparent ceramic sheet (3) and blue-light LED chip (2), described sheet of transparent ceramic (3) and described LED chip (2) are fixed on support, the chemical formula of described cerium dopping yttrium aluminum garnet transparent ceramic sheet (3) material is: (Y
1-xce
x)
3al
5o
12, 0.0005≤x≤0.005 in formula.
2. crystalline ceramics white light LEDs according to claim 1, is characterized in that the preparation method of described cerium dopping yttrium aluminum garnet transparent ceramic sheet (3) is as follows:
According to chemical formula (Y
1-xce
x)
3al
5o
12metering yttrium salt, aluminium salt and cerium salt, with deionized water dissolving and mix, be mixed with Al by yttrium salt, aluminium salt and cerium salt
3+concentration is the mixing salt solution of 0.1mol/L～0.2mol/L; By NH
4hCO
3be dissolved in alcohol-water double solvents preparation NH
4hCO
3concentration is the precipitant solution of 0.5mol/L～2mol/L, and the volume ratio of described ethanol and water is 0.5:1～1.2:1; Described mixing salt solution is titrated in described precipitant solution at normal pressure, 10 ℃～20 ℃, and titration finishes rear ageing at least 10 hours, then, through vacuum filtration, washing, oven dry, obtains presoma; Described presoma, 1100～1250 ℃ of roastings 2～3 hours, is obtained to cerium doped yttrium aluminum garnet powder; Described cerium doped yttrium aluminum garnet powder is formed to biscuit through dry-pressing formed and isostatic cool pressing, then biscuit is put in vacuum sintering furnace 1700～1780 ℃ of sintering at least 10 hours, obtain cerium dopping yttrium aluminum garnet transparent ceramic sheet.
3. crystalline ceramics white light LEDs according to claim 2, is characterized in that described yttrium salt is Y (NO
3)
3or YCl
3, described aluminium salt is NH
4al (SO
4)
2or Al (NO
3)
3, described cerium salt is Ce (NO
3)
3.
4. according to the crystalline ceramics white light LEDs described in arbitrary claim in claims 1 to 3, the thickness that it is characterized in that described cerium dopping yttrium aluminum garnet transparent ceramic sheet (3) is 0.1mm～1.0mm.
Priority Applications (1)
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| CN103205254B (en) * | 2013-04-10 | 2015-09-16 | 中国科学院福建物质结构研究所 | Comprise white light LEDs of New Solid transparent fluorescent material and preparation method thereof |
| CN104505449A (en) * | 2014-12-16 | 2015-04-08 | 福建中科芯源光电科技有限公司 | Large-power white-light LED (light emitting diode) and encapsulated method thereof |
| CN112005049B (en) * | 2018-03-29 | 2023-02-28 | 昕诺飞控股有限公司 | Single sided illumination for high lumen density lamps |
| CN108997014A (en) * | 2018-09-28 | 2018-12-14 | 成都东骏激光股份有限公司 | A kind of high color fluorescent ceramics and the preparation method and application thereof |
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| CN102136541A (en) * | 2010-01-22 | 2011-07-27 | 中国科学院上海硅酸盐研究所 | Transparent ceramic white-light LED (Light-Emitting Diode) device |
| CN102338307A (en) * | 2010-07-19 | 2012-02-01 | 惠州元晖光电有限公司 | Phosphor coating films and lighting apparatuses using the same |
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| CN101899301A (en) * | 2010-06-25 | 2010-12-01 | 海洋王照明科技股份有限公司 | LED light-emitting material, LED light-emitting device and manufacturing method |
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