CN104818024A - White LED comprising novel solid-state transparent fluorescent material and preparing method thereof - Google Patents

White LED comprising novel solid-state transparent fluorescent material and preparing method thereof Download PDF

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Publication number
CN104818024A
CN104818024A CN201510198165.9A CN201510198165A CN104818024A CN 104818024 A CN104818024 A CN 104818024A CN 201510198165 A CN201510198165 A CN 201510198165A CN 104818024 A CN104818024 A CN 104818024A
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transparent
fluor
fluorescent material
crystalline ceramics
chip
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CN104818024B (en
Inventor
曹永革
刘著光
邓种华
郭旺
李军庭
陈剑
陈东川
兰海
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Fujian Institute of Research on the Structure of Matter of CAS
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Fujian Institute of Research on the Structure of Matter of CAS
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/10—Bump connectors; Manufacturing methods related thereto
    • H01L2224/12—Structure, shape, material or disposition of the bump connectors prior to the connecting process
    • H01L2224/14—Structure, shape, material or disposition of the bump connectors prior to the connecting process of a plurality of bump connectors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/10—Bump connectors; Manufacturing methods related thereto
    • H01L2224/15—Structure, shape, material or disposition of the bump connectors after the connecting process
    • H01L2224/16—Structure, shape, material or disposition of the bump connectors after the connecting process of an individual bump connector
    • H01L2224/161—Disposition
    • H01L2224/16151—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
    • H01L2224/16221—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/16225—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being non-metallic, e.g. insulating substrate with or without metallisation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/42—Wire connectors; Manufacturing methods related thereto
    • H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
    • H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
    • H01L2224/4805—Shape
    • H01L2224/4809—Loop shape
    • H01L2224/48091—Arched
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/15—Details of package parts other than the semiconductor or other solid state devices to be connected
    • H01L2924/161—Cap
    • H01L2924/1615—Shape
    • H01L2924/16195—Flat cap [not enclosing an internal cavity]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

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Abstract

The invention provides transparent fluorescence, particularly transparent ceramic fluorescence, transparent glass fluorescence and transparent composite fluorescence, and a white LED comprising the three types of transparent fluorescence. The fluorescent powder in the traditional white LED light source is replaced with the transparent fluorescent material, and the white LED is obtained. The transparent fluorescence has the advantages of high heat conductivity, high stability and high crystallinity; color temperature drift of the white LED light source caused by high temperature is avoided; stability of the white LED light source is improved; luminous efficacy of the white LED light source is improved.

Description

Comprise white light LEDs of New Solid transparent fluorescent material and preparation method thereof
Technical field
The invention provides a kind of transparent fluorescent material, especially crystalline ceramics fluor, transparent glass fluor and transparent composite fluorescence body, and apply the white light LEDs of these three kinds of transparent phosphor.
Background technology
Photodiode (Light Emitting Diode-LED) can be directly luminous energy electric energy conversion.LED chip is made up of two portions, and a part is P-type semiconductor, and inside it, occupy an leading position in hole, and the other end is N-type semiconductor, mainly electronics.When these two kinds of semi-conductors couple together time, between them, just form one " P-N junction ".When electric current acts on this wafer by wire time, electronics will be pushed to P district, and in P district, electronics is with hole-recombination, then will send energy with the form of photon, the principle of LED luminescence that Here it is.
LED is as a kind of new type light source, and owing to having energy-saving and environmental protection, the life-span is long, toggle speed fast, can control luminescent spectrum and forbid being with the size of width to make the unrivaled advantage of the more high conventional light source of colorfulness and obtain unprecedented development.
Generally speaking, LED has two kinds of main method producing white light usually, and a kind of is use three monochrome photodiodes launching red, green, blue, and colour mixture forms white light.Another kind uses fluorescent material to convert the monochromatic ray that blue or ultraviolet LED send the white light of wide spectrum to.The white light that wherein, a kind of method produces is mainly used in Large Screen Display Technology, and the white light that then a kind of method produces is mainly used in illumination and backlight.
For rear a kind of white light technology, Ya company of Japan has the pioneer invention (US5998925A) in this field: adopt blue GaN chip excite YAG yellow fluorescent powder and obtain white light, the inventive point of this patent is yttrium aluminium garnet fluorescent powder, this fluorescent material absorbs 450nm to 470nm wavelength blue light, excite and produce 550nm to 560nm wavelength gold-tinted, there is the advantage that cost is low, efficiency is high.But for common blue light or UV LED chip, its photoelectric transformation efficiency is generally lower than 30%, even LED chip best at present, its photoelectric transformation efficiency also can not higher than 50%.Therefore LED will supervene a large amount of heat when luminescence.The general chip circumference lighted, temperature can arrive 150 degrees Celsius to 200 degrees Celsius.Such temperature will cause the decrease in efficiency 20-30% of fluorescent material, thus produce the colour temperature of light source and the skew of chromaticity coordinates.Also have impact on light efficiency and the stability of LED light source simultaneously.And the temperature of yttrium aluminum garnet (YAG) fluorescent material more than 120 degrees Celsius can be degenerated, simultaneously because the phosphor material powder of coating is non-transparent material, the light that blue light or ultraviolet chip send by time can there is the phenomenons such as scattering absorption, make light extraction efficiency not high; Simultaneously because the uneven meeting of applied thickness has a strong impact on its hot spot and white light colour temperature.Such as owing to applying the problems such as uneven yellow light ring, blue hot spot, the white light colour temperature caused be inconsistent.
Summary of the invention
The present invention is intended to the foregoing problems solving prior art, there is provided a kind of structure simple, the fluorescent ceramic material of the high and dependable performance of light efficiency and comprise the LED chip of this stupalith, and utilize the luminous fluorescence excitation pottery of LED chip, produce the preparation method of the white light LEDs of white light, a kind of White-light LED chip structure is also provided simultaneously.
The present invention is achieved through the following technical solutions:
One, transparent fluorescent material
The invention provides a kind of crystalline ceramics fluor, the technical scheme comprising following aspect:
(1) a crystalline ceramics fluor, is characterized in that, described fluor has following chemical formula: Re 3al 5o 12, wherein rare earth element Re is selected from Ce, a kind of or several arbitrarily mixture in Eu, Er, Nd, Tb, Sm, Tm, Dy, Y, Gd, Pr, Lu, Ho, Pm, La or Yb.
(2) according to the crystalline ceramics fluor of (1), it is characterized in that, the straight line transmittance of described transparent phosphor within the scope of 250nm-480nm is greater than 5%, preferred transmitance is for being greater than 50%, straight line transmittance within the scope of 480nm-780nm is greater than 5%, and preferred transmitance is for being greater than 80%.
(3) according to the crystalline ceramics fluor of (1) or (2), it is characterized in that, the peak wavelength of described crystalline ceramics phosphor excitation spectrum is within the scope of 250nm-480nm, and the peak wavelength of emission spectrum is within the scope of 480-780nm.
(4) according to the crystalline ceramics fluor of any one of (1)-(3), it is characterized in that, the thickness of described crystalline ceramics fluor is 0.5-2mm.
(5) according to the crystalline ceramics fluor of any one of (1)-(4), it is characterized in that, described crystalline ceramics fluor can be prepared as sheet, box-like, hemispherical etc. as required.
The present invention also provides the preparation method of the one as above crystalline ceramics fluor of any one of (1)-(5), and it comprises following technical scheme:
(6) preparation method for crystalline ceramics fluor, is characterized in that, described method comprises the steps:
A. powder preparation: by Re 3al 5o 12stoichiometric ratio weigh Al 2o 3with Re 2o 3powder, and add certain sintering aid, binding agent, softening agent, dispersion agent,
Wherein said Re is rare earth element.
According to the present invention, described Re 2o 3powder is selected from Ce 2o 3, Eu 2o 3, Er 2o 3, Nd 2o 3, Tb 2o 3, Sm 2o 3, Tm 2o 3, Dy 2o 3, Y 2o 3, Gd 2o 3, Pr 2o 3, Lu 2o 3, Ho 2o 3, Pm 2o 3, La 2o 3or Yb 2o 3in the mixture of one or more;
B. biscuit of ceramics is shaping: fluorescence ceramics powder raw material step (1) obtained, by traditional wet method or dry-press process, makes biscuit after drying.
C. binder removal: calcined by the High Temperature Furnaces Heating Apparatus that the biscuit that step (2) obtains puts into 900-1500 DEG C, the time is 20min-20h, to discharge the organic component in biscuit;
D. sinter: the biscuit of ceramics of step (4) is put into high temperature sintering furnace and sinters, described sintering temperature is 800-2100 DEG C, and preferable temperature is 1000-1900 DEG C, more preferably 1200-1850 DEG C, and temperature rise rate is 0.5-10 DEG C/min.Sintering time 2-20 hour, preferably: 12-30 hour;
E. anneal: the pottery after sintering densification is put into annealing furnace and carries out anneal, annealing temperature is 900-1500 DEG C, and preferable temperature is 1200 DEG C-1500 DEG C, and annealing time is 1h-20h.Temperature rise rate is 0.5-10 DEG C/min.
According to the present invention, described sintering aid is MgO or CaO or TEOS or SiO 2, addition is described Al 2o 3with Re 2o 30 ~ 2wt% of mixed powder quality, preferred 0.5-1wt%.
According to the present invention, described binding agent be selected from polyvinyl butyral acetal, polyoxyethylene glycol, polyvinyl alcohol, Sudan Gum-arabic, marine alga acid amide, methylcellulose gum, Walocel MT 20.000PV, ethyl cellulose, Natvosol, Methacrylamide, methylene-bisacrylamide, hydroxypropylcellulose, polyoxyethylene one or more.
According to the present invention, the addition of described binding agent is 0.1 ~ 10% of above-mentioned mixed oxidization amount.
According to the present invention, described softening agent be selected from lipid acid, polyvalent alcohol, fatty acid ester, citric acid fat, polyester plasticizer, epoxy plasticizer one or more.
According to the present invention, the addition of described softening agent is 0.1 ~ 10% of mixed oxidization amount.
According to the present invention, described dispersion agent be selected from polyacrylic acid, polypropylene, polypropylene amine, polyethylene, polyvinylidene, polyoxyethylene glycol, Sudan Gum-arabic, gelatin, menhaden fish oil, fish oil, oleic acid, Viscotrol C one or more.
According to the present invention, the addition of described dispersion agent regulates consumption according to the size of original powder.
According to the present invention, the forming method of described step (2) comprises traditional dry pressing, isostatic pressing method, casting method, slip casting method, teeming practice, extrusion molding, injection moulding and gel casting forming method etc.
The present invention also provides a kind of transparent glass fluor, and it comprises following technical scheme:
(1) a transparent glass fluor, is characterized in that, the molar percentage of described transparent glass fluor consists of:
AF, BF 2, A 2the mixture of one or more in O or BO: 0-25%;
Re 2o 3or ReF 3in the mixture of one or more: 0.001-25%;
Al 2O 3：20-40％；
SiO 2：20-70％；
Wherein A is selected from basic metal Li, Na, K, Rb, Cs;
B is selected from alkaline-earth metal Be, Mg, Ca, Sr, Ba;
Re is selected from rare earth element: one or more in Ce, Eu, Er, Nd, Tb, Sm, Tm, Dy, Y, Gd, Pr, Lu, Ho, Pm, La or Yb.
(2) according to the transparent glass fluor of (1), it is characterized in that, the straight line transmittance of described fluor within the scope of 250nm-480nm is greater than 5%, preferred transmitance is greater than 50%, straight line transmittance within the scope of 480nm-780nm is greater than 5%, and preferred transmitance is greater than 80%.
(3) according to the transparent glass fluor of (1) or (2), it is characterized in that, the peak wavelength of described transparent glass phosphor excitation spectrum is within the scope of 250nm-480nm, and the peak wavelength of emission spectrum is within the scope of 480-780nm.
(4) according to the transparent glass fluor of any one of (1)-(3), it is characterized in that, the thickness of described transparent glass fluor is 0.5-2mm.
(5) according to the transparent glass fluor of any one of (1)-(4), it is characterized in that, the shape of described transparent glass fluor is sheet, box-like, hemispherical etc.
The present invention also provides the preparation method of the transparent glass fluor of any one of above-mentioned (1)-(5), and it comprises following technical scheme:
(6) preparation method of the transparent glass fluor of any one of a kind of above-mentioned (1)-(5), it is characterized in that, described method comprises the steps:
Formula by the molar percentage of any one of above-mentioned (1)-(5):
AF, BF 2, A 2the mixture of one or more in O or BO: 0-20%;
Re 2O 3：0.001-25％、Al 2O 3：21-40％；
SiO 2: 25-70%, raw materials weighing,
Pour in crucible after raw material is mixed and melt, glass melting temperature 1400-1700 DEG C, be incubated and after 2-15 hour, glass melt poured on pig mold, then be placed in High Temperature Furnaces Heating Apparatus to anneal, annealing temperature is 400-1500 DEG C, and annealing time is 2-10 hour, then cools to room temperature with the furnace.
The present invention also provides a kind of transparent composite fluorescence body, and it comprises following technical scheme:
(1) a kind of transparent composite fluorescence body, it is characterized in that, described fluor is matrix material, comprise above-mentioned crystalline ceramics fluor and transparent glass fluor, the mass ratio of wherein said crystalline ceramics fluor and transparent glass fluor is: 45:55 ~ 95:5, preferred 60:40 ~ 80:20.
According to composite fluorescence body of the present invention, described crystalline ceramics fluor proportion is 45-95%, is preferably 60%-90%, is more preferably 70%-80%.
(2) the transparent composite fluorescence body Gen Ju (1), it is characterized in that this transparent composite fluorescence body is the rhythmo structure of crystalline ceramics fluor and transparent glass fluor, the thickness of bi-material is respectively 0.5-2mm.
(3) the transparent composite fluorescence body Gen Ju (1) or (2), is characterized in that, the stimulated emission spectrum of described transparent composite fluorescence body can contain whole visible-range, i.e. 380-780nm, preferred 480-780nm.
(4) according to the transparent composite fluorescence body of any one of (1)-(3), it is characterized in that, the straight line transmittance of described fluor within the scope of 250nm-480nm is greater than 5%, preferred transmitance is for being greater than 50%, straight line transmittance within the scope of 480nm-780nm is greater than 5%, and preferred transmitance is for being greater than 80%.
(5) according to the transparent composite fluorescence body of any one of (1)-(4), it is characterized in that, the shape of described transparent composite fluorescence body is sheet, box-like or hemispherical etc.
(6) the present invention also provides the preparation method of the transparent composite fluorescence body of any one of above-mentioned (1)-(3), and it is characterized in that, described method comprises the steps:
A. prepare crystalline ceramics fluor, its preparation process is as described in crystalline ceramics fluor.
B. by the formula molar percentage raw materials weighing of described glass fluor, pour in crucible after raw material is mixed and melt, glass melting temperature 1400-1700 DEG C, is incubated and pours on pig mold by glass melt after 2-15 hour, and the bottom of this pig mold placed the ceramic phosphor that above-mentioned preparation completes.Then entirety is placed in High Temperature Furnaces Heating Apparatus to anneal, annealing temperature is 400-1500 DEG C, and annealing time is 2-10 hour, then cools to room temperature with the furnace, and the demoulding also obtains transparent composite fluorescence body.
The present invention also provides a kind of crystalline ceramics fluor for the application of white light LEDs, it is characterized in that, described crystalline ceramics fluor is described above.
The present invention also provides a kind of transparent glass fluor for the application of white light LEDs, and it is characterized in that, transparent glass fluor is described above.
The present invention also provides a kind of transparent composite fluorescence body for the application of white light LEDs, and it is characterized in that, transparent composite fluorescence body is described above.
Two, the white light LEDs of transparent phosphor is applied
1, a kind of white-light LED encapsulation light source applying transparent fluorescent material
The invention provides a kind of white-light LED encapsulation light source applying fluorescent material, comprise following technical scheme:
(1) a kind of white-light LED encapsulation light source applying transparent fluorescent material, comprise base plate for packaging 12, the blue light of more than one or ultraviolet leds chip 20 and transparent fluorescent material 11, it is characterized in that, described transparent fluorescent material 11 is selected from crystalline ceramics fluor as aforesaid in the present invention, transparent glass fluor and transparent composite fluorescence body.
According to the present invention, described transparent fluorescent material 11 is positioned at the topmost of packaged light source.
According to the present invention, described blue light or ultraviolet leds chip 20 are positioned at the top of base plate for packaging 12, are fixed on base plate for packaging 12 by silica gel or elargol (being commercially available) 50.The electrode 30 that described chip 20 and frame bottom are installed is connected.
According to the present invention, described transparent fluorescent material 11 covers on blue light or ultraviolet leds chip 20.Preferably, described transparent fluorescent material 11 is fixed on base plate for packaging 12 by transparent colloid 40 (being commercially available) with described chip 20.
(2) according to the white-light LED encapsulation light source of above-mentioned (1), it is characterized in that: described in the optical excitation transparent fluorescent material 11 utilizing blue light or UV LED chip 20 to send, transparent fluorescent material 11 is selected from crystalline ceramics fluor as aforesaid in the present invention, transparent glass fluor and transparent composite fluorescence body.
In the present invention, transparent fluorescent material instead of the use of fluorescent material in Conventional white LED, and the optical excitation fluorescent material sent by chip 20 forms white light.
(3) according to the white-light LED encapsulation light source of above-mentioned (1) or (2), it is characterized in that: the emmission spectrum of described LED chip 20 is peak wavelength in the visible ray of 400-500nm or the peak wavelength UV-light at 250-400nm.
(4) according to the white-light LED encapsulation light source of any one of above-mentioned (1)-(3), it is characterized in that: described LED chip can be vertical stratification, horizontal structure and inverted structure LED chip.
2, a kind of double-side LED light source applying transparent fluorescent material
The present invention also provides a kind of double-side LED light source applying transparent fluorescent material, and it comprises following technical scheme:
(1) a kind of white-light LED encapsulation light source applying transparent fluorescent material, comprise the blue light of transparent fluorescent material base plate for packaging more than 10, or ultraviolet leds chip 20 and transparent fluorescent material 11, it is characterized in that described transparent fluorescent material base plate for packaging 10 is selected from crystalline ceramics fluor as aforesaid in the present invention, transparent glass fluor and transparent composite fluorescence body with transparent fluorescent material 11.
According to the present invention, described blue light or ultraviolet leds chip 20 are positioned at the top of base plate for packaging 10, are fixed on base plate for packaging 10 by transparent colloid (being commercially available) 51.The electrode 30 that described chip 20 and frame bottom are installed is connected.
According to the present invention, described transparent fluorescent material 11 covers on blue light or ultraviolet leds chip 20.Preferably, described transparent fluorescent material 11 is fixed on base plate for packaging 12 by transparent colloid 40 (being commercially available) with described chip 20.
(2) according to the white-light LED encapsulation light source of above-mentioned (1), it is characterized in that, the front and back of described LED chip 20 all can be luminous.
According to the present invention, the light sent by LED chip 20 back side through transparent fluorescent material substrate 10 directly this LED encapsulation structure of injection, thus can define the LED light source of a tow sides luminescence.
(3) according to the white-light LED encapsulation light source of above-mentioned (1) or (2), it is characterized in that, the optical excitation utilizing blue light or UV LED chip 20 to send is positioned at the transparent fluorescent material base plate for packaging 10 at its back side and is positioned at the transparent fluorescent material 11 in its front, described transparent fluorescent material 10 and 11 is selected from crystalline ceramics fluor as aforesaid in the present invention, transparent glass fluor and transparent composite fluorescence body.
In the present invention, transparent fluorescent material instead of the use of fluorescent material in Conventional white LED, and the optical excitation fluorescent material sent by chip 20 forms white light, thus makes transparent fluorescent material instead of the use of fluorescent material in Conventional white LED.
(4) according to the white-light LED encapsulation light source of any one of above-mentioned (1)-(3), it is characterized in that, the emmission spectrum of described LED chip is peak wavelength in the visible ray of 400-500nm or the peak wavelength UV-light at 250-400nm.
(5) according to the white-light LED encapsulation light source of any one of above-mentioned (1)-(4), it is characterized in that: described LED chip is selected from horizontal structure, vertical stratification or inverted structure LED chip.
The present invention utilizes the fluorescent material in transparent phosphor replacement conventional white light LED light source, white light LEDs.Because transparent phosphor has the advantage of high thermal conductance, high stability and high-crystallinity, the color temperature shift avoiding white LED light source to cause due to high temperature, improves the stability of white LED light source, and improves the light efficiency of white LED light source.
Accompanying drawing illustrates:
Fig. 1 is the white-light LED encapsulation light source that embodiment 1,3,5 applies crystalline ceramics fluor;
Fig. 2 is the (Ce of embodiment 1 0.06%y 99.94%) 3al 5o 12xRD figure spectrum after crystalline ceramics fluor sintering;
Fig. 3 is the spectrum of the white LED light source of embodiment 1;
Fig. 4 is the white-light LED encapsulation light source that embodiment 2 applies transparent glass fluor;
Fig. 5 is the spectrum of the white LED light source of embodiment 2;
Fig. 6 is the (Ce of embodiment 3 0.06%gd 10%y 89.94%) 3al 5o 12xRD figure spectrum after crystalline ceramics fluor sintering;
Fig. 7 is the spectrum of the white LED light source of embodiment 3;
Fig. 8 is the white-light LED encapsulation light source that embodiment 4 applies transparent composite fluorescence body;
Fig. 9 is the spectrum of the white LED light source of embodiment 4;
Figure 10 is the (Ce of embodiment 5 0.1%gd 10%y 29.9%tb 60%) 3al 5o 12xRD figure spectrum after crystalline ceramics fluor sintering;
Figure 11 is the spectrum of the white LED light source of embodiment 5;
Figure 12 is the white-light LED encapsulation light source of embodiment 6;
Figure 13 is the (Ce of embodiment 6 0.06%y 99.94%) 3al 5o 12xRD figure spectrum after crystalline ceramics fluor sintering;
Figure 14 is the spectrum of the white LED light source of embodiment 6;
Figure 15 is the white-light LED encapsulation light source of embodiment 7;
Figure 16 is the spectrum of the white LED light source of embodiment 7;
Figure 17 is the white LED light source of embodiment 8;
Figure 18 is the (Ce of embodiment 8 0.06%y 99.94%) 3al 5o 12xRD figure spectrum after crystalline ceramics fluor sintering;
Figure 19 is the spectrum of the white LED light source of embodiment 8;
Figure 20 is the white LED light source of embodiment 9;
Figure 21 is the spectrum of the white LED light source of embodiment 9;
Figure 22 is the white LED light source of embodiment 10;
Figure 23 is the spectrum of the white LED light source of embodiment 10;
Embodiment
The present invention is described in detail by following embodiment.But those skilled in the art understand, and following embodiment is not limiting the scope of the invention, any improvement of making on basis of the present invention and change are all within protection scope of the present invention.
Embodiment 1
By (Ce 0.06%y 99.94%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, Ce 2o 3powder raw material, mixed powder adds the TEOS of 0.1200g, and the polyvinyl butyral acetal of 0.5400g puts into high purity agate jar, adds high-purity agate ball of 80g, dehydrated alcohol 12g, and ball milling puts into the dry 15h of baking oven after 20 hours.With the powder sieving powder after mortar grinder and obtain 45 ~ 75 μm, use the unidirectional pressurization of the forcing spindle of 10Mpa respectively, after being pressed into former, isostatic cool pressing under 200Mpa.900 DEG C of binder removals 20 hours at ambient pressure, and the biscuit after binder removal is sintered in a vacuum, temperature rise rate is 10 DEG C/min, sintering temperature is 1850 DEG C, temperature rise rate is 10 DEG C/min, and sintering time is 15 hours, and the sample after sintering was through 1500 DEG C of annealing 10 hours, finally carry out polishing to sample, the thickness of sample after polishing is 0.64mm.Visible light transmissivity can reach 83%.Fig. 2 is (Ce 0.06%y 99.94%) 3al 5o 12xRD figure spectrum after crystalline ceramics fluor sintering, each peak position in figure and Re 3al 5o 12the standard peak position of ceramic garnet phase matches, and not assorted peak, illustrate that this sample changes garnet phase into completely through this sintering process.
As shown in Figure 1, utilize the LED chip 20 that peak wavelength is 460nm by commercial silica gel 50 to be fixed on the die bond position of aluminium oxide ceramic substrate 12, baking makes silica gel 50 solidify in an oven.The electrode of LED chip 20 is connected with the electrode 30 of aluminium oxide ceramic substrate 12 by recycling gold thread.Last transparent silica gel 40 on chip 20 location point of aluminium oxide ceramic substrate 12 also covers crystalline ceramics fluor 11, and baking makes transparent silica gel 40 solidify in an oven.The photoelectricity test result of this white LED light source is: colour temperature is Tc=5261K, colour rendering index Ra=69.5, light efficiency η=91lm/W.The spectrogram of its test as shown in Figure 3.
Embodiment 2
Following powder body material is weighed by table 1 molar percentage:
Table 1
Raw material NaF MgO Ce 2O 3 Y 2O 3 Al 2O 3 SiO 2
Component (mol%) 5％ 2％ 2％ 20％ 35％ 36％
Raw material is poured in platinum crucible after ball milling mixes and melts, glass melting temperature 1650 DEG C, being incubated poured on pig mold by glass melt after 2 hours, then be placed in High Temperature Furnaces Heating Apparatus to anneal, annealing temperature is 750 DEG C, and annealing time 2 hours, then cools to room temperature with the furnace, obtain transparent glass fluor, thickness is 0.8mm.
As shown in Figure 4, utilize the LED chip 20 that peak wavelength is 460nm by commercial silica gel 50 to be fixed on the die bond position of aluminium oxide ceramic substrate 12, baking makes silica gel 50 solidify in an oven.The electrode of LED chip 20 is connected with the electrode 30 of aluminium oxide ceramic substrate 12 by recycling gold thread.Last transparent silica gel 40 on chip 20 location point of aluminium oxide ceramic substrate 12 also covers transparent glass fluor 13, and baking makes transparent silica gel 40 solidify in an oven.The photoelectricity test result of this white LED light source is: colour temperature is Tc=5400K, colour rendering index Ra=69, light efficiency η=83lm/W.The spectrogram of its test as shown in Figure 5.
Embodiment 3
By (Ce 0.06%gd 10%y 89.94%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, Gd 2o 3with Ce 2o 3powder raw material, mixed powder adds the TEOS of 0.1200g, and the polyvinyl butyral acetal of 0.5400g puts into high purity agate jar, adds high-purity agate ball of 80g, dehydrated alcohol 12g, and ball milling puts into the dry 15h of baking oven after 20 hours.With the powder sieving powder after mortar grinder and obtain 45 ~ 75 μm, use the unidirectional pressurization of the forcing spindle of 10Mpa respectively, after being pressed into former, isostatic cool pressing under 200Mpa.1500 DEG C of binder removals 20 minutes at ambient pressure, and the biscuit after binder removal is sintered in a vacuum, temperature rise rate is 10 DEG C/min, and sintering temperature is 1200 DEG C, and sintering time is 20h.Sample after sintering was through 1500 DEG C of annealing 1 hour, and finally carry out polishing to sample, the thickness of sample after polishing is 0.66mm.Visible light transmissivity can reach 81%.Fig. 6 is (Ce 0.06%gd 10%y 89.94%) 3al 5o 12xRD figure spectrum after crystalline ceramics fluor sintering, each peak position in figure and Re 3al 5o 12the standard peak position of ceramic garnet phase matches, and not assorted peak, illustrate that this sample changes garnet phase into completely through this sintering process.
As shown in Figure 1, utilize the LED chip 20 that peak wavelength is 460nm by commercial silica gel 50 to be fixed on the die bond position of aluminium oxide ceramic substrate 12, baking makes silica gel 50 solidify in an oven.The electrode of LED chip 20 is connected with the electrode 30 of aluminium oxide ceramic substrate 12 by recycling gold thread.Last transparent silica gel 40 on chip 20 location point of aluminium oxide ceramic substrate 12 also covers crystalline ceramics fluor 11, and baking makes transparent silica gel 40 solidify in an oven.The photoelectricity test result of this white LED light source is: colour temperature is Tc=4561K, colour rendering index Ra=75.5, light efficiency η=85lm/W.The spectrogram of its test as shown in Figure 7.
Embodiment 4
The first step: by (Ce 0.06%gd 10%y 89.94%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, Gd 2o 3with Ce 2o 3powder raw material, mixed powder adds the TEOS of 0.1200g, and the polyvinyl butyral acetal of 0.5400g puts into high purity agate jar, adds high-purity agate ball of 80g, dehydrated alcohol 12g, and ball milling puts into the dry 15h of baking oven after 20 hours.With the powder sieving powder after mortar grinder and obtain 45 ~ 75 μm, use the unidirectional pressurization of the forcing spindle of 10Mpa respectively, after being pressed into former, isostatic cool pressing under 200Mpa.1500 DEG C of binder removals 20 hours at ambient pressure, and the biscuit after binder removal is sintered in a vacuum, temperature rise rate is 10 DEG C/min, and sintering temperature is 1800 DEG C, and sintering time is 15h.Thickness of sample after polishing is 0.66mm.
Second step: weigh following powder body material by table 2 molar percentage:
Table 2
Raw material LiF GdF3 PrF3 Al2O3 SiO2
Component (mol%) 20％ 19％ 1％ 20％ 40％
Raw material is poured in platinum crucible after ball milling mixes and melts, glass melting temperature 1700 DEG C, be incubated and after 15 hours, glass melt poured on pig mold, place at (Ce prepared by the first step in advance in pig mold 0.06%gd 10%y 89.94%) 3al 5o 12crystalline ceramics fluor.Then entirety is placed in High Temperature Furnaces Heating Apparatus to anneal, annealing temperature is 1500 DEG C, and annealing time 10 hours, then cools to room temperature with the furnace, obtains transparent composite fluorescence body, and thickness is 0.7mm.
3rd step: as shown in Figure 8, utilizes the LED chip 20 that peak wavelength is 455nm by commercial silica gel 50 to be fixed on the die bond position of aluminium oxide ceramic substrate 12, and baking makes silica gel 50 solidify in an oven.The electrode of LED chip 20 is connected with the electrode 30 of aluminium oxide ceramic substrate 12 by recycling gold thread.Last transparent silica gel 40 on chip 20 location point of aluminium oxide ceramic substrate 12 also covers transparent composite fluorescence body 14, and baking makes transparent silica gel 40 solidify in an oven.The photoelectricity test result of this white LED light source is: colour temperature is Tc=3543K, colour rendering index Ra=85.6, light efficiency η=80lm/W.The spectrogram of its test as shown in Figure 9.
Embodiment 5
By (Ce 0.1%gd 10%y 29.9%tb 60%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Tb 2o 3powder, Y 2o 3powder, Gd 2o 3with Ce 2o 3powder raw material, mixed powder adds the SiO2 of 0.1500g, and the polyoxyethylene glycol of 0.8000g and the mixture of methylcellulose gum put into high purity agate jar, adds high-purity agate ball of 80g, dehydrated alcohol 12g, and ball milling puts into the dry 15h of baking oven after 20 hours.With the powder sieving powder after mortar grinder and obtain 45 ~ 75 μm, use the unidirectional pressurization of the forcing spindle of 10Mpa respectively, after being pressed into former, isostatic cool pressing under 200Mpa.1300 DEG C of binder removals 5 hours at ambient pressure, and the biscuit after binder removal is sintered in a vacuum, temperature rise rate is 0.5 DEG C/min, and sintering temperature is 1200 DEG C, and sintering time is 20h.Sample after sintering is through 1200 DEG C of annealing, and temperature rise rate is 10 DEG C/min, and annealing time is 20 hours, finally carries out polishing to sample, and the thickness of sample after polishing is 0.66mm.Visible light transmissivity can reach 81%.Figure 10 is (Ce 0.1%gd 10%y 29.9%tb 60%) 3al 5o 12xRD figure spectrum after crystalline ceramics fluor sintering, each peak position in figure and Re 3al 5o 12the standard peak position of ceramic garnet phase matches, and not assorted peak, illustrate that this sample changes garnet phase into completely through this sintering process.
As shown in Figure 1, utilize the LED chip 20 that peak wavelength is 460nm by commercial silica gel 50 to be fixed on the die bond position of aluminium oxide ceramic substrate 12, baking makes silica gel 50 solidify in an oven.The electrode of LED chip 20 is connected with the electrode 30 of aluminium oxide ceramic substrate 12 by recycling gold thread.Last transparent silica gel 40 on chip 20 location point of aluminium oxide ceramic substrate 12 also covers the crystalline ceramics fluor 11 that above-mentioned preparation completes, and baking makes transparent silica gel 40 solidify in an oven.The photoelectricity test result of this white LED light source is: colour temperature is Tc=6561K, colour rendering index Ra=65.5, light efficiency η=85lm/W.The spectrogram of its test as shown in figure 11.
Embodiment 6
By (Ce 0.06%y 99.94%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, Ce 2o 3powder raw material, mixed powder adds the TEOS of 0.2400g, and the PVB of 0.5400g puts into high purity agate jar, adds high-purity agate ball of 160g, dehydrated alcohol 24g, and ball milling puts into the dry 15h of baking oven after 20 hours.With the powder sieving powder after mortar grinder and obtain 45 ~ 75 μm, use the unidirectional pressurization of the forcing spindle of 10Mpa respectively, after being pressed into former, isostatic cool pressing under 200Mpa.1300 DEG C of binder removals 10 hours at ambient pressure, and the biscuit after binder removal is sintered in a vacuum, temperature rise rate is 10 DEG C/min, sintering temperature is 1850 DEG C, sintering time is 15 hours, sample after sintering was through 1600 DEG C of annealing 10 hours, and finally carry out polishing to sample, the thickness of sample after polishing is 0.64mm.Visible light transmissivity can reach 82%.Figure 13 is (Ce 0.06%y 99.94%) 3al 5o 12xRD figure spectrum after crystalline ceramics fluor sintering, each peak position in figure and Re 3al 5o 12the standard peak position of ceramic garnet phase matches, and not assorted peak, illustrate that this sample changes garnet phase into completely through this sintering process.
As shown in figure 12, utilize the LED chip 20 that peak wavelength is 460nm by commercial clear silica gel 51 to be fixed on the die bond position of crystalline ceramics fluor 10, baking makes transparent silica gel 51 solidify in an oven.The electrode of LED chip 20 is connected with the electrode 30 of crystalline ceramics fluor 10 by recycling gold thread.Last transparent silica gel 40 on chip 20 location point of crystalline ceramics fluor 10 also covers crystalline ceramics fluor 11, and baking makes transparent silica gel 40 solidify in an oven.The photoelectricity test result of this white LED light source is: colour temperature is Tc=5179K, colour rendering index Ra=69.3, light efficiency η=151lm/W.The spectrogram of its test as shown in figure 14.
Embodiment 7
The first step: by (Ce 0.06%gd 10%y 89.94%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, Gd 2o 3with Ce 2o 3powder raw material, mixed powder adds the TEOS of 0.2400g, and Sudan Gum-arabic and the marine alga acid amide of 1.0800g put into high purity agate jar, add high-purity agate ball of 160g, dehydrated alcohol 24g, and ball milling puts into the dry 15h of baking oven after 20 hours.With the powder sieving powder after mortar grinder and obtain 45 ~ 75 μm, use the unidirectional pressurization of the forcing spindle of 10Mpa respectively, after being pressed into former, isostatic cool pressing under 200Mpa.1500 DEG C of binder removals 20 hours at ambient pressure, and the biscuit after binder removal is sintered in a vacuum, temperature rise rate is 10 DEG C/min, and sintering temperature is 1600 DEG C, and sintering time is 18h.Thickness of sample after polishing is 0.66mm.
Second step: weigh following powder body material by table 4 molar percentage:
Table 4
Raw material LiF GdF 3 PrF 3 Al 2O 3 SiO 2
Component (mol%) 20％ 19％ 1％ 20％ 40％
Raw material is poured in platinum crucible after ball milling mixes and melts, glass melting temperature 1700 DEG C, be incubated and after 15 hours, glass melt poured on pig mold, place at (Ce prepared by the first step in advance in pig mold 0.06%gd 10%y 89.94%) 3al 5o 12crystalline ceramics fluor.Then entirety is placed in High Temperature Furnaces Heating Apparatus to anneal, annealing temperature is 1500 DEG C, and annealing time 10 hours, then cools to room temperature with the furnace, obtains composite transparent fluor, and thickness is 0.83mm.
3rd step:
As shown in figure 15, utilize the LED chip 20 that peak wavelength is 455nm by commercial clear silica gel 51 to be fixed on the die bond position of transparent composite fluorescence body 15, baking makes silica gel 51 solidify in an oven.The electrode of LED chip 20 is connected with the electrode 30 of aluminium oxide ceramic substrate 12 by recycling gold thread.Last transparent silica gel 40 on chip 20 location point of aluminium oxide ceramic substrate 12 also covers transparent composite fluorescence body 14, and baking makes transparent silica gel 40 solidify in an oven.The photoelectricity test result of this white LED light source is: colour temperature is Tc=3723K, colour rendering index Ra=87.6, light efficiency η=131lm/W.The spectrogram of its test as shown in figure 16.
Embodiment 8
The first step:
By (Ce 0.06%y 99.94%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, Ce 2o 3powder raw material, mixed powder adds the TEOS of 0.2400g, and the PVB of 0.5400g puts into high purity agate jar, adds high-purity agate ball of 160g, dehydrated alcohol 24g, and ball milling puts into the dry 15h of baking oven after 20 hours.With the powder sieving powder after mortar grinder and obtain 45 ~ 75 μm, use the unidirectional pressurization of the forcing spindle of 10Mpa respectively, after being pressed into former, isostatic cool pressing under 200Mpa.1300 DEG C of binder removals 10 hours at ambient pressure, and the biscuit after binder removal is sintered in a vacuum, temperature rise rate is 10 DEG C/min, sintering temperature is 1800 DEG C, sintering time is 15 hours, sample after sintering was through 1250 DEG C of annealing 10 hours, and finally carry out polishing to sample, the thickness of sample after polishing is 0.64mm.Visible light transmissivity can reach 83%.Figure 18 is (Ce 0.06%y 99.94%) 3al 5o 12xRD figure spectrum after crystalline ceramics fluor sintering, each peak position in figure and Re 3al 5o 12the standard peak position of ceramic garnet phase matches, and not assorted peak, illustrate that this sample changes garnet phase into completely through this sintering process.
Second step: by (Ce 0.06%y 99.94%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, Ce 2o 3powder raw material, add the MgO sintering aid of 0.5at%, 0.5wt% dispersion agent gathers volatile salt, 15wt% Methacrylamide (MAM) organic monomer, 1:20 is (organic monomer: linking agent) N doubly, N '-methylene-bisacrylamide (MBAM), 0.8wt% softening agent polyvinyl alcohol (PEG), 0.5wt% defrother propyl carbinol; Raw material, abrading-ball, additive are poured into 36 grams of deionized water ball millings and mixed 24 hours, rotational speed of ball-mill 350r/m, material: ball=1:5.Mixed for ball milling slurry interpolation 0.5wt% initiator ammonium persulfate (APS) and 0.1wt% catalyzer Tetramethyl Ethylene Diamine (TEMED) are put into vacuum tank, vacuum-treat reaches below-0.1Mpa to vacuum tightness, till not having bubble to overflow in slurry.Slurry after de-bubble injects mould, and put into 60 DEG C of baking oven trigger monomer reactions, wait slurry solidify in place base substrate to be separated with mould, the demoulding, the green compact after shaping have the shape of crystalline ceramics fluor 16 in Figure 13.Shaping green compact are dry stage by stage to 100 DEG C from room temperature, initial setting temperature 30 DEG C, humidity 90%, slowly increase temperature minimizing humidity and are slowly raised to 100 DEG C.Dried green compact are put into tube furnace and be warmed up to 700 DEG C with 1 DEG C/min temperature rise rate under oxygen atmospheres, and be incubated 2 hours, oxygen flow is per minute 50 ~ 100ml, with stove naturally cooling after insulation terminates.Vacuum oven put into by green compact after degreasing, under vacuum atmosphere, (vacuum tightness 1.5 × 10-4Pa) sinters, 1200 DEG C are raised to 10 DEG C/min temperature rise rate, then be warming up to 1830 DEG C with 5 DEG C/min temperature rise rate and be incubated 20 hours at 1830 DEG C, 1200 DEG C are dropped to 5 DEG C/min rate of temperature fall, naturally cool to room temperature, obtain the crystalline ceramics fluor 16 in Figure 17.
3rd step: as shown in figure 17, utilizes LED chip 20 that peak wavelength is 450nm by commercial clear silica gel to be fixed on the centre of the crystalline ceramics fluor 10 that step one preparation completes, and baking makes transparent silica gel solidify in an oven.Again the crystalline ceramics fluor 16 prepared through step 2 is overlying on above chip, and applies transparent colloid and chip 20 and ceramic phosphor are bondd and put into baking box solidify.The photoelectricity test result of this white LED light source is: colour temperature is Tc=5389K, colour rendering index Ra=70.3, light efficiency η=151lm/W.The spectrogram of its test as shown in figure 19.
Embodiment 9
The first step: by (Ce 0.06%gd 10%y 89.94%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, Gd 2o 3with Ce 2o 3powder raw material, mixed powder adds the TEOS of 0.1200g, and the PVB of 0.5400g puts into high purity agate jar, adds high-purity agate ball of 80g, dehydrated alcohol 12g, and ball milling puts into the dry 15h of baking oven after 20 hours.With the powder sieving powder after mortar grinder and obtain 45 ~ 75 μm, use the unidirectional pressurization of the forcing spindle of 10Mpa respectively, after being pressed into former, isostatic cool pressing under 200Mpa.900 DEG C of binder removals 20 hours at ambient pressure, and the biscuit after binder removal is sintered in a vacuum, temperature rise rate is 10 DEG C/min, and sintering temperature is 1800 DEG C, and sintering time is 15h.Sample after sintering was through 1200 DEG C of annealing 20 hours, and finally carry out polishing to sample, the thickness of sample after polishing is 0.66mm.
Second step: by (Ce 0.06%gd 10%y 89.94%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, Gd 2o 3with Ce 2o 3powder raw material, add the MgO sintering aid of 0.5at%, 0.5wt% dispersion agent gathers volatile salt, 15wt% Methacrylamide (MAM) organic monomer, 1:20 is (organic monomer: linking agent) N doubly, N '-methylene-bisacrylamide (MBAM), 0.8wt% softening agent polyvinyl alcohol (PEG), 0.5wt% defrother propyl carbinol; Raw material, abrading-ball, additive are poured into 36 grams of deionized water ball millings and mixed 24 hours, rotational speed of ball-mill 350r/m, material: ball=1:5.Mixed for ball milling slurry interpolation 0.5wt% initiator ammonium persulfate (APS) and 0.1wt% catalyzer Tetramethyl Ethylene Diamine (TEMED) are put into vacuum tank, vacuum-treat reaches below-0.1Mpa to vacuum tightness, till not having bubble to overflow in slurry.Slurry after de-bubble injects mould, and put into 60 DEG C of baking oven trigger monomer reactions, wait slurry solidify in place base substrate to be separated with mould, the demoulding, the green compact after shaping have the shape of crystalline ceramics fluor 16 in Figure 13.Shaping green compact are dry stage by stage to 100 DEG C from room temperature, initial setting temperature 30 DEG C, humidity 90%, slowly increase temperature minimizing humidity and are slowly raised to 100 DEG C.Dried green compact are put into tube furnace and be warmed up to 700 DEG C with 1 DEG C/min temperature rise rate under oxygen atmospheres, and be incubated 2 hours, oxygen flow is per minute 50 ~ 100ml, with stove naturally cooling after insulation terminates.Vacuum oven put into by green compact after degreasing, under vacuum atmosphere, (vacuum tightness 1.5 × 10-4Pa) sinters, 1200 DEG C are raised to 10 DEG C/min temperature rise rate, then be warming up to 1830 DEG C with 5 DEG C/min temperature rise rate and be incubated 20 hours at 1830 DEG C, 1200 DEG C are dropped to 5 DEG C/min rate of temperature fall, naturally cool to room temperature, obtain the crystalline ceramics fluor 16 in Figure 20.
Peak wavelength is that the inverted structure LED chip 20 of 455nm utilizes eutectic welding technology to be welded on the pad 30 of crystalline ceramics fluor 10 prepared by the above-mentioned the first step by the 3rd step: as shown in figure 20.Again the crystalline ceramics fluor 16 prepared through second step is overlying on above chip 20, and utilizes transparent silica gel chip 20 and ceramic phosphor to be bondd and put into baking box to solidify.The photoelectricity test result of this white LED light source is: colour temperature is Tc=4561K, colour rendering index Ra=75.5, light efficiency η=165lm/W.The spectrogram of its test as shown in figure 21.
Embodiment 10
The first step: by (Ce 0.06%gd 10%y 89.94%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, Gd 2o 3with Ce 2o 3powder raw material, mixed powder adds the TEOS of 0.1200g, and the PVB of 0.5400g puts into high purity agate jar, adds high-purity agate ball of 80g, dehydrated alcohol 12g, and ball milling puts into the dry 15h of baking oven after 20 hours.With the powder sieving powder after mortar grinder and obtain 45 ~ 75 μm, use the unidirectional pressurization of the forcing spindle of 10Mpa respectively, after being pressed into former, isostatic cool pressing under 200Mpa.900 DEG C of binder removals 20 hours at ambient pressure, and the biscuit after binder removal is sintered in a vacuum, temperature rise rate is 10 DEG C/min, and sintering temperature is 1800 DEG C, and sintering time is 15h.Sample after sintering was through 1200 DEG C of annealing 20 hours, and finally carry out polishing to sample, the thickness of sample after polishing is 0.66mm.
Second step: by (Ce 0.06%gd 10%y 89.94%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, Gd 2o 3with Ce 2o 3powder raw material, add the MgO sintering aid of 0.5at%, 0.5wt% dispersion agent gathers volatile salt, 15wt% Methacrylamide (MAM) organic monomer, 1:20 is (organic monomer: linking agent) N doubly, N '-methylene-bisacrylamide (MBAM), 0.8wt% softening agent polyvinyl alcohol (PEG), 0.5wt% defrother propyl carbinol; Raw material, abrading-ball, additive are poured into 36 grams of deionized water ball millings and mixed 24 hours, rotational speed of ball-mill 350r/m, material: ball=1:5.Mixed for ball milling slurry interpolation 0.5wt% initiator ammonium persulfate (APS) and 0.1wt% catalyzer Tetramethyl Ethylene Diamine (TEMED) are put into vacuum tank, vacuum-treat reaches below-0.1Mpa to vacuum tightness, till not having bubble to overflow in slurry.Slurry after de-bubble injects mould, and put into 60 DEG C of baking oven trigger monomer reactions, wait slurry solidify in place base substrate to be separated with mould, the demoulding, the green compact after shaping have the shape of crystalline ceramics fluor 16 in Figure 13.Shaping green compact are dry stage by stage to 100 DEG C from room temperature, initial setting temperature 30 DEG C, humidity 90%, slowly increase temperature minimizing humidity and are slowly raised to 100 DEG C.Dried green compact are put into tube furnace and be warmed up to 700 DEG C with 1 DEG C/min temperature rise rate under oxygen atmospheres, and be incubated 2 hours, oxygen flow is per minute 50 ~ 100ml, with stove naturally cooling after insulation terminates.Vacuum oven put into by green compact after degreasing, under vacuum atmosphere, (vacuum tightness 1.5 × 10-4Pa) sinters, 1200 DEG C are raised to 10 DEG C/min temperature rise rate, then be warming up to 1830 DEG C with 5 DEG C/min temperature rise rate and be incubated 20 hours at 1830 DEG C, 1200 DEG C are dropped to 5 DEG C/min rate of temperature fall, naturally cool to room temperature, obtain the crystalline ceramics fluor 17 in Figure 22.
Peak wavelength is that the inverted structure LED chip 20 of 455nm utilizes eutectic welding technology to be welded on the pad 30 of crystalline ceramics fluor 10 prepared by the above-mentioned the first step by the 3rd step: as shown in figure 22.Again the crystalline ceramics fluor 16 prepared through second step is overlying on above chip 20, and utilizes transparent silica gel chip 20 and ceramic phosphor to be bondd and put into baking box to solidify.The photoelectricity test result of this white LED light source is: colour temperature is Tc=4561K, colour rendering index Ra=75.5, light efficiency η=165lm/W.The spectrogram of its test as shown in figure 23.

Claims (10)

1. a crystalline ceramics fluor, is characterized in that, described fluor chemical formula is Re 3al 5o 12, wherein rare earth element Re is selected from Ce, a kind of or several arbitrarily mixture in Eu, Er, Nd, Tb, Sm, Tm, Dy, Y, Gd, Pr, Lu, Ho, Pm, La or Yb.
Preferably, the straight line transmittance of described transparent phosphor within the scope of 250nm-480nm is greater than 5%, and preferred transmitance is for being greater than 50%, and the straight line transmittance within the scope of 480nm-780nm is greater than 5%, and preferred straight line transmittance is greater than 80%.
Preferably, the peak wavelength of described crystalline ceramics phosphor excitation spectrum is within the scope of 250nm-480nm, and the peak wavelength of emission spectrum is within the scope of 480-780nm.
Preferably, described crystalline ceramics fluor can be sheet, box-like, hemispherical.
Preferably, the thickness of described crystalline ceramics fluor is 0.5-2mm.
2. crystalline ceramics fluor according to claim 1, is characterized in that, the chemical formula of described crystalline ceramics fluor is selected from
(Ce 0.06％Y 99.94％) 3Al 5O 12；
(Ce 0.06%gd 10%y 89.94%) 3al 5o 12; Or
(Ce 0.1％Gd 10％Y 29.9％Tb 60％) 3Al 5O 12。
3. a preparation method for the crystalline ceramics fluor of any one of claim 1-2, is characterized in that adopting the preparation method comprised the following steps:
A. powder preparation: by Re 3al 5o 12stoichiometric ratio weigh Al 2o 3with Re 2o 3powder, and add certain sintering aid, binding agent, softening agent, dispersion agent, described Re 2o 3powder is selected from Ce 2o 3, Eu 2o 3, Er 2o 3, Nd 2o 3, Tb 2o 3, Sm 2o 3, Tm 2o 3, Dy 2o 3, Y 2o 3, Gd 2o 3, Pr 2o 3, Lu 2o 3, Ho 2o 3, Pm 2o 3, La 2o 3or Yb 2o 3in the mixture of one or more;
B. biscuit of ceramics is shaping: fluorescence ceramics powder raw material step (1) obtained is by traditional wet method or dry-press process, make biscuit after drying, wherein forming method comprises traditional dry pressing, isostatic pressing method, casting method, slip casting method, teeming practice, extrusion molding, injection moulding and gel casting forming method;
C. binder removal: calcined by the High Temperature Furnaces Heating Apparatus that the biscuit that step (2) obtains puts into 900-1500 DEG C, the time is 20min-20h, to discharge the organic component in biscuit;
D. sinter: again biscuit of ceramics is put into high temperature sintering furnace and sinter, described sintering temperature is 800-2100 DEG C, and temperature rise rate is 0.5-10 DEG C/min; Sintering time 2-20 hour;
E. anneal: the pottery after sintering densification is put into annealing furnace and carries out anneal, annealing temperature is 900-1500 DEG C; Annealing time is 1h-20h; Temperature rise rate is 0.5-10 DEG C/min.
4. preparation method according to claim 3, is characterized in that, described sintering temperature is 1000-1900 DEG C, and described sintering time is 12-30 hour; Described annealing temperature is 1200 DEG C-1500 DEG C.
Preferably, described sintering temperature is 1200-1850 DEG C.
5., according to the preparation method of any one of claim 3-4, it is characterized in that,
Described sintering aid is MgO or CaO or TEOS or SiO 2, addition is described Al 2o 3with Re 2o 30 ~ 2wt% of mixed powder quality; Preferred 0.5-1wt%.
Described binding agent be selected from polyvinyl butyral acetal, polyoxyethylene glycol, polyvinyl alcohol, Sudan Gum-arabic, marine alga acid amide, methylcellulose gum, Walocel MT 20.000PV, ethyl cellulose, Natvosol, Methacrylamide, methylene-bisacrylamide, hydroxypropylcellulose, polyoxyethylene one or more; The addition of described binding agent is 0.1 ~ 10% of above-mentioned mixed oxidization amount;
Described softening agent be selected from lipid acid, polyvalent alcohol, fatty acid ester, citric acid fat, polyester plasticizer, epoxy plasticizer one or more, the addition of described softening agent is 0.1 ~ 10% of mixed oxidization amount;
Described dispersion agent be selected from polyacrylic acid, polypropylene, polypropylene amine, polyethylene, polyvinylidene, polyoxyethylene glycol, Sudan Gum-arabic, gelatin, menhaden fish oil, fish oil, oleic acid, Viscotrol C one or more.
Preferably, the addition of described sintering aid is described Al 2o 3with Re 2o 3the 0.5-1wt% of mixed powder quality.
6. a transparent composite fluorescence body, it comprises a kind of crystalline ceramics fluor described in any one of claim 1-2 and transparent glass fluor as described below,
The molar percentage of described transparent glass fluor consists of:
AF, BF 2, A 2the mixture of one or more in O or BO: 0-25%;
Re 2o 3or ReF 3in the mixture of one or more: 0.001-25%;
Al 2O 3：20-40％；
SiO 2：20-70％；
Wherein A is selected from basic metal Li, Na, K, Rb, Cs;
B is selected from alkaline-earth metal Be, Mg, Ca, Sr, Ba;
Re is selected from rare earth element: one or more in Ce, Eu, Er, Nd, Tb, Sm, Tm, Dy, Y, Gd, Pr, Lu, Ho, Pm, La or Yb;
It is characterized in that, this transparent composite fluorescence body is the rhythmo structure of crystalline ceramics fluor and transparent glass fluor, and the thickness of bi-material is respectively 0.5-2mm.
Preferably, the stimulated emission spectrum of described transparent composite fluorescence body can contain whole visible-range, i.e. 380-780nm, preferred 480-780nm.
Preferably, the straight line transmittance of described transparent composite fluorescence body within the scope of 250nm-480nm is greater than 5%, and preferred transmitance is for being greater than 50%, and the straight line transmittance within the scope of 480nm-780nm is greater than 5%, and preferred transmitance is for being greater than 80%.
7. transparent composite fluorescence body according to claim 6, is characterized in that, described transparent glass fluor is selected from:
NaF:5%; MgO:2%; Ce 2o 32%; Y 2o 3: 20%; Al 2o 3: 35%; SiO 2: 36%, or
LiF：20％；GdF 3：19％；PrF 3：1％；Al 2O 3：20％；SiO 2：40％。
8. the crystalline ceramics fluor of an any one of claim 1-4 is used for the application of white light LEDs.
9. apply the white-light LED encapsulation light source of transparent fluorescent material for one kind, comprise base plate for packaging 12, the blue light of more than one or ultraviolet leds chip 20 and transparent fluorescent material 11, it is characterized in that, described transparent fluorescent material 11 is selected from the crystalline ceramics fluor of any one of claim 1-4, and the transparent composite fluorescence body of any one of claim 16-20.
Preferably, described transparent fluorescent material 11 is positioned at the topmost of packaged light source.
Preferably, described blue light or ultraviolet leds chip 20 are positioned at the top of base plate for packaging 12, are fixed on base plate for packaging 12 by silica gel or elargol 50, and the electrode 30 that described chip 20 and frame bottom are installed is connected.
Preferably, described transparent fluorescent material 11 covers on blue light or ultraviolet leds chip 20.
Preferably, described transparent fluorescent material 11 is fixed on base plate for packaging 12 by transparent colloid 40 with described chip 20.
10. apply the double-side LED light source of transparent fluorescent material for one kind, comprise transparent fluorescent material base plate for packaging 10, the blue light of more than one or ultraviolet leds chip 20 and transparent fluorescent material 11, it is characterized in that described transparent fluorescent material base plate for packaging 10 and transparent fluorescent material 11 are selected from the crystalline ceramics fluor of any one of claim 1-2, with the transparent composite fluorescence body of any one of claim 6-7, described encapsulating structure makes the light sent by LED chip front and the back side be mixed to white light via transparent fluorescent material base plate for packaging 10 and transparent fluorescent material 11 respectively, form the white light LEDs of a dual emission white light.
Preferably, described blue light or ultraviolet leds chip 20 are positioned at the top of base plate for packaging 10, are fixed on base plate for packaging 10 by transparent colloid 51.The electrode 30 that described chip 20 and frame bottom are installed is connected.
Preferably, described transparent fluorescent material 11 covers on blue light or ultraviolet leds chip 20.Preferably, described transparent fluorescent material 11 is fixed on transparent fluorescent material base plate for packaging 10 by transparent colloid 40 with described chip 20.
Preferably, the front and back of described LED chip 20 all can be luminous.
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