CN1306628C - Process for making white light diode by using blue light or purple light emitting diode chips - Google Patents
Process for making white light diode by using blue light or purple light emitting diode chips Download PDFInfo
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- CN1306628C CN1306628C CNB200410018651XA CN200410018651A CN1306628C CN 1306628 C CN1306628 C CN 1306628C CN B200410018651X A CNB200410018651X A CN B200410018651XA CN 200410018651 A CN200410018651 A CN 200410018651A CN 1306628 C CN1306628 C CN 1306628C
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Abstract
The present invention relates to a method for preparing diodes emitting white light by diode wafers capable of emitting blue light or purple light. The present invention is characterized in that the method comprises the following steps: fixing diode wafers capable of emitting blue light or purple light to the bottom of a reaction container; adding proportionally prepared water solutions of yttrium acetate and europium acetate at the temperature of 80 to 85 DEG C and the pH value of the solution from 4 to 6, and dropping a water solution of isobutanol aluminium under the condition of stirring; continually stirring until that gelatin is formed on the surfaces of the diode wafers after the water solution of isobutanol aluminium is dropped; taking out after the materials are sintered for 40 minutes at the temperature from 850 DEG C to 1100 DEG C for cutting and encapsulating to make the diode emitting white light. The present invention has the advantages that the sintering temperature of the fluorescent powder is low because of a wet method in order to cause yttrium aluminum garnet films on the surfaces of the wafers to have the advantages of small granularity, compaction, large adhesion force, even film thickness and flat and smooth film surfaces; the luminous quality of diodes emitting white light is enhanced, the yield is as high as 90%, the steps for preparing films are reduced, and the process loss of materials is low for further reducing the production cost of diodes emitting white light.
Description
Technical field
The present invention relates to a kind of preparation method of light-emitting diode, relate in particular to the method that a kind of diode wafer that adopts blue light-emitting or purple light prepares white-light emitting diode.
Background technology
The development of advancing by leaps and bounds along with semi-conducting material, the appearance of a new generation's light-emitting diode, as new type light source, its power consumption only is 1/10 of an ordinary incandescent lamp, and the life-span can prolong 100 times, owing to have advantages such as energy-conservation, long-life, non-maintaining, environmental protection, thereby to replace traditional incandescent lamp and fluorescent lamp be trend of the times, especially white-light emitting diode can be widely used in display application such as domestic lighting, road traffic illumination, automotive lighting, landscape light in city and aviation, harbour, station, stadiums, advertising media because of it, thereby market prospects are wide.But at present, the general preparation method of commercially available luminescent pigment optical diode is the method that adopts solid synthetic, concrete step is that the europium yttrium aluminium garnet fluorescent powder is mixed in preparation earlier, the diode wafer surface of it being sized mixing spraying to blue light-emitting or purple light then, again through adding the heat abstraction solvent, and itself and diode wafer are solidified togather, mix the europium yttrium aluminium garnet fluorescent powder through blue light or purple light excited send amber light and with the synthetic white light that produces of blue light or purple light.The shortcoming of this method is a sintering temperature height in the preparation process of mixing europium iridium aluminium garnet fluorescent material, and generally more than 1600-1700 ℃, thereby the granularity of the fluorescent material that forms is big, diameter reaches 5-15 μ m, and adhesive force is not strong, and membrane thickness unevenness, rate of finished products is low, and general qualification rate is lower than 70%; In addition, adopt the solid synthetic method to need sintering powder process, combine the twice heating process with LED wafer curing again, technical process is complicated, and in the fluorescent powder jet printing process, owing to adopt single LED wafer spraying method, fluorescent material may spray and drop on outside the LED wafer, thereby the fluorescent material waste is big, and these have all strengthened manufacturing cost.
Summary of the invention
The objective of the invention is to problem at above-mentioned existence, it is the aqueous chemical synthetic method is made white-light emitting diode at the diode wafer surface attachment yttrium-aluminium-garnet rete of blue light-emitting or purple light method that a kind of wet method that adopts is provided, compare with above-mentioned solid synthetic method, sintering temperature is low in its rete forming process, the granularity that forms is little, adhesive force is big, fluorescent film thickness is even, and film surface is smooth smooth, luminous mass and rate of finished products height; Film making process reduces; The utilance of material improves, and can further reduce the production cost of white-light emitting diode, thereby overcome above-mentioned defective.
Technical scheme of the present invention has provided the method that a kind of diode wafer that adopts blue light-emitting or purple light prepares white-light emitting diode, it is characterized in that being made of following operation:
(1) preparation yttrium acetate, the acetate europium aqueous solution, with molar ratio computing, yttrium acetate is 0.997～0.980, and the acetate europium is 0.003～0.02, and water is 80～100; After taking by weighing material, under 80-85 ℃ of temperature, yttrium acetate, acetate europium added and make yttrium acetate, the acetate europium aqueous solution in the entry;
(2) the preparation isobutanol aluminum aqueous solution with molar ratio computing, is 3 by the total amount of yttrium acetate and acetate europium in aqueous solution of preparation in (1), and dry isobutanol aluminium amount is 5, take by weighing material after, be 1 with dry isobutanol aluminium again, water is 80～100 to take by weighing the water yield; Under 80-85 ℃ of temperature, dry isobutanol aluminium added then and make the aqueous solution in the entry;
(3) in contained yttrium acetate, acetate europium and isobutanol aluminum gross mass in the aqueous solution of (1) and (2) preparation, by 1 gram: 20cm
2The diode wafer ratio diode wafer of getting blue light-emitting or purple light put into reaction vessel and be fixed on reaction container bottom, then, the temperature that (1) is made is that 80-85 ℃ yttrium acetate, the acetate europium aqueous solution joins in the reaction vessel, keeping temperature is 80-85 ℃, the solution pH value is 4-6 and stirs the existence dropping isobutanol aluminum aqueous solution down, drip off the back and continue to stir till the diode wafer surface forms gel, then diode wafer is taken out;
(4) blue light-emitting of the surface attachment gel layer that takes out or the diode wafer of purple light are put into baking furnace, heating up in the dehydration back, forms europkium-activated yttrium-aluminium-garnet rete on 40 minutes top layers of 850 ℃ of-1100 ℃ of following sintering;
(5) (4) are made with the diode wafer of the europkium-activated yttrium-aluminium-garnet rete package lead again of cutting into slices according to a conventional method, be the white-light emitting diode finished product.
In this method, isobutanol aluminum and yttrium acetate, the acetate europium has been realized the even mixing on ion concentration between the ion in solution, carrying out along with polymerization reaction in the solution, product is piled up thickening and even diode wafer surface attached to blue light-emitting or purple light gradually, because the activity function of ion itself improves greatly, thereby the temperature of the polymer of synthesizing stable is significantly reduced, above-mentioned gel can generate at 850-1100 ℃ mixes the europium yag crystal, proportioning by above-mentioned reactant and LED wafer surface area, what light-emitting diode can obtain 20-25 μ m thickness mixes europium yttrium-aluminium-garnet rete, compare with the synthetic separately solid sintering of mixing the europium yttrium aluminium garnet fluorescent powder of employing solid process, shake off solid and just can mutually combine together because of the ion in its various solids at first will at high temperature obtain enough energy its constraint, so need 1600-1700 ℃ high temperature, cause the big performance of granularity bad, and employing this method, because granularity is little, fine and close, the strong adhesion difficult drop-off, and carry out with reaction, polymer is piled layer by layer to build and is attached to the LED wafer surface, therefore thicknesses of layers is even, and surfacing is smooth.
Advantage of the present invention is: owing to adopted the wet method manufacturing, the fluorescent material sintering temperature is reduced, the yttrium-aluminium-garnet rete granularity that the diode wafer surface forms is little, fine and close, adhesive force is big, and thicknesses of layers is even, and film surface is smooth smooth, improved the luminous mass of white-light emitting diode, the rate of finished products height can reach 90%, and film making process reduces, the process loss of material is low, has further reduced the production cost of white-light emitting diode.
Embodiment
Below be elaborated by the preparation method of specific embodiment to the diode wafer of employing blue light-emitting provided by the invention or purple light.
Embodiment 1
(1) preparation yttrium acetate, the acetate europium aqueous solution, with molar ratio computing, yttrium acetate is 0.997, and the acetate europium is 0.003, and water is 80; Take by weighing and analyze pure yttrium acetate 17.079 grams, analyze pure acetate europium 0.061 gram, water 72.700 grams add yttrium acetate, acetate europium under 80-85 ℃ of temperature and make yttrium acetate, the acetate europium aqueous solution in the entry;
(2) the preparation isobutanol aluminum aqueous solution with molar ratio computing, is 3 by the total amount of yttrium acetate and acetate europium in aqueous solution of preparation in (1), dry isobutanol aluminium amount is 5, take by weighing analyze pure dry isobutanol aluminium 20.707 grams after, be 1 with dry isobutanol aluminium again, water is 80, takes by weighing water 121.200 grams; Under 80-85 ℃ of temperature, dry isobutanol aluminium added then and make the aqueous solution in the entry;
(3) in contained yttrium acetate, acetate europium and isobutanol aluminum gross mass in the aqueous solution of (1) and (2) preparation, by 1 gram: 20cm
2The diode wafer ratio to get 10 specifications be 4 * 5cm
2The diode wafer of blue light-emitting put into reaction vessel and the holddown groove by the bottom is fixed on reaction container bottom, then, the temperature that (1) is made is 80-85 ℃ a yttrium acetate, the acetate europium aqueous solution joins in the reaction vessel, keeping solution temperature is 80-85 ℃, the solution pH value is 4-6 and stirs the existence dropping isobutanol aluminum aqueous solution down, dripping off the back continues to stir till all diode wafer surfaces form gel, then diode wafer is taken out, solution temperature will remain on 80-85 ℃ in this process, and available acetate regulator solution pH value remains on 4-6.
(4) 10 blue light-emitting diode wafers of the surface attachment gel layer that takes out are put into baking furnace, heating up in the dehydration back, forms europkium-activated yttrium-aluminium-garnet rete on 40 minutes top layers of 850 ℃ of following sintering;
(5) 10 blue light-emitting diode wafers with europkium-activated yttrium-aluminium-garnet rete of (4) being made take out, and according to a conventional method, are cooled to room temperature, distinguish package lead again after all cutting into 2000 with every, are the white-light emitting diode finished product.
10 blue light-emitting diode wafers that form europkium-activated yttrium-aluminium-garnet top layer are tested piecewise: through using the X-ray diffraction map analysis, the amorphous state gel on 10 diode wafer surfaces peak value all occurred at 850 ℃, illustrates to have formed europkium-activated yttrium-aluminium-garnet crystalline phase; Observe the luminescent spectrum with cathode-ray exciting, main peak appears at 592 ± 2nm scope, and with the chromascope test, color coordinates distribution is in X=0.534 ± 0.005, and Y=0.453 ± 0.005 scope is amber; With the luminance meter test, Luminance Distribution is in 14 ± 0.5FL scope; Get europkium-activated yttrium-aluminium-garnet layer thickness profile at the 20-21 mu m range with the thickness instrumentation, thicknesses of layers is even; Amplify 1900 times of test particle size diameters between 1-2 μ m with electron microscope, and film surface is smooth smooth, above-mentioned all Performance Detection explanation index reaches qualified finished product requirement; After cutting the wafer that amounts to 20,000 white-light emitting diodes is detected piecewise, draw " * " trace with the test nail at film surface, 91% no marking meets the requirements.
Embodiment 2
(1) preparation yttrium acetate, the acetate europium aqueous solution, with molar ratio computing, yttrium acetate is 0.990, and the acetate europium is 0.010, and water is 90; Take by weighing and analyze pure yttrium acetate 16.857 grams, analyze pure acetate europium 0.201 gram, water 81.300 grams add yttrium acetate, acetate europium under 80-85 ℃ of temperature and make yttrium acetate, the acetate europium aqueous solution in the entry;
(2) the preparation isobutanol aluminum aqueous solution with molar ratio computing, is 3 by the total amount of yttrium acetate and acetate europium in aqueous solution of preparation in (1), dry isobutanol aluminium amount is 5, take by weighing analyze pure dry isobutanol aluminium 20.568 grams after, be 1 with dry isobutanol aluminium again, water is 90, takes by weighing water 135.400 grams; Under 80-85 ℃ of temperature, dry isobutanol aluminium added then and make the aqueous solution in the entry;
(3) in contained yttrium acetate, acetate europium and isobutanol aluminum gross mass in the aqueous solution of (1) and (2) preparation, by 1 gram: 20cm
2The diode wafer ratio to get 10 specifications be 4 * 5cm
2Purple-light illuminanted diode wafer put into reaction vessel and the holddown groove by the bottom is fixed on reaction container bottom, then, the temperature that (1) is made is 80-85 ℃ a yttrium acetate, the acetate europium aqueous solution joins in the reaction vessel, keeping solution temperature is 80-85 ℃, the solution pH value is 4-6 and stirs the existence dropping isobutanol aluminum aqueous solution down, dripping off the back continues to stir till all diode wafer surfaces form gel, then diode wafer is taken out, solution temperature will remain on 80-85 ℃ in this process, and available acetate regulator solution pH value remains on 4-6.
(4) 10 blue optical diode wafers of the surface attachment gel layer that takes out are put into baking furnace, heating up in the dehydration back, forms europkium-activated yttrium-aluminium-garnet rete on 40 minutes top layers of 1000 ℃ of following sintering;
That (5) (4) are made takes out with the blue optical diode wafers of 10 of europkium-activated yttrium-aluminium-garnet rete, according to a conventional method, is cooled to room temperature, distinguishes package lead again after all cutting into 2000 with every, is the white-light emitting diode finished product.
10 blue optical diode wafers that form europkium-activated yttrium-aluminium-garnet top layer are tested piecewise: through using the X-ray diffraction map analysis, the amorphous state gel on 10 diode wafer surfaces peak value occurs at 1000 ℃, formed europkium-activated yttrium-aluminium-garnet crystalline phase, but, illustrate that crystallization is more complete than more sharp at the peak value of 850 ℃ of appearance; Observe the luminescent spectrum with cathode-ray exciting, main peak appears at 592 ± 2nm scope, and with the chromascope test, color coordinates distribution is in X=0.534 ± 0.005, and Y=0.453 ± 0.005 scope is amber; With the luminance meter test, Luminance Distribution is in 18 ± 0.5FL scope; Get europkium-activated yttrium-aluminium-garnet layer thickness profile at the 22-23 mu m range with the thickness instrumentation, thicknesses of layers is even; Amplify 1900 times of test particle size diameters between 1-3 μ m with electron microscope, and film surface is smooth smooth, above-mentioned all Performance Detection explanation index reaches qualified finished product requirement; After cutting the wafer that amounts to 20,000 white-light emitting diodes is detected piecewise, draw " * " trace with the test nail at film surface, 91% no marking meets the requirements.
Embodiment 3
(1) preparation yttrium acetate, the acetate europium aqueous solution, with molar ratio computing, yttrium acetate is 0.980, and the acetate europium is 0.020, and water is 100; Take by weighing and analyze pure yttrium acetate 16.538 grams, analyze pure acetate europium 0.398 gram, water 89.600 grams add yttrium acetate, acetate europium under 80-85 ℃ of temperature and make yttrium acetate, the acetate europium aqueous solution in the entry;
(2) the preparation isobutanol aluminum aqueous solution with molar ratio computing, is 3 by the total amount of yttrium acetate and acetate europium in aqueous solution of preparation in (1), dry isobutanol aluminium amount is 5, take by weighing analyze pure dry isobutanol aluminium 20.398 grams after, be 1 with dry isobutanol aluminium again, water is 100, takes by weighing water 149.200 grams; Under 80-85 ℃ of temperature, dry isobutanol aluminium added then and make the aqueous solution in the entry;
(3) in contained yttrium acetate, acetate europium and isobutanol aluminum gross mass in the aqueous solution of (1) and (2) preparation, by 1 gram: 20cm
2The diode wafer ratio to get 10 specifications be 4 * 5cm
2The diode wafer of blue light-emitting put into reaction vessel and the holddown groove by the bottom is fixed on reaction container bottom, then, the temperature that (1) is made is 80-85 ℃ a yttrium acetate, the acetate europium aqueous solution joins in the reaction vessel, keeping solution temperature is 80-85 ℃, the solution pH value is 4-6 and stirs the existence dropping isobutanol aluminum aqueous solution down, dripping off the back continues to stir till all diode wafer surfaces form gel, then diode wafer is taken out, solution temperature will remain on 80-85 ℃ in this process, and available acetate regulator solution pH value remains on 4-6.
(4) 10 blue light-emitting diode wafers of the surface attachment gel layer that takes out are put into baking furnace, heating up in the dehydration back, forms europkium-activated yttrium-aluminium-garnet rete on 40 minutes top layers of 1100 ℃ of following sintering;
(5) 10 blue light-emitting diode wafers with europkium-activated yttrium-aluminium-garnet rete of (4) being made take out, and according to a conventional method, are cooled to room temperature, distinguish package lead again after all cutting into 2000 with every, are the white-light emitting diode finished product.
10 blue light-emitting diode wafers that form europkium-activated yttrium-aluminium-garnet top layer are tested piecewise: through using the X-ray diffraction map analysis, the amorphous state gel on 10 diode wafer surfaces peak value occurs for 1100 ℃, formed europkium-activated yttrium-aluminium-garnet crystalline phase, but, illustrate that crystallization is purer than sharper at the peak value of 1000 ℃ of appearance; Observe the luminescent spectrum with cathode-ray exciting, main peak appears at 592 ± 2nm scope, and with the chromascope test, color coordinates distribution is in X=0.534 ± 0.005, and Y=0.453 ± 0.005 scope is amber; With the luminance meter test, Luminance Distribution is in 17 ± 0.4FL scope; Get europkium-activated yttrium-aluminium-garnet layer thickness profile at the 24-25 mu m range with the thickness instrumentation, thicknesses of layers is even; Amplify 1900 times of test particle size diameters between 1-5 μ m with electron microscope, illustrate with temperature to raise that the rete granularity increases, but the surface is still more smooth smooth, above-mentioned all Performance Detection explanation index reaches qualified finished product requirement; After cutting the wafer that amounts to 20,000 white-light emitting diodes is detected piecewise, draw " * " trace with the test nail at film surface, 90% no marking meets the requirements.
In the above-described embodiments, embodiment 2 is a most preferred embodiment.
Used in the present embodiment yttrium acetate, acetate europium, dry isobutanol aluminum chemistry reagent, blue light-emitting and blue optical diode wafer all can be purchased on market.
Claims (1)
1, a kind of diode wafer that adopts blue light-emitting or purple light prepares the method for white-light emitting diode, it is characterized in that being made of following operation:
(1), preparation yttrium acetate, the acetate europium aqueous solution, with molar ratio computing, yttrium acetate is 0.997～0.980, the acetate europium is 0.003～0.02, water is 80～100; After taking by weighing material, under 80-85 ℃ of temperature, yttrium acetate, acetate europium added and make yttrium acetate, the acetate europium aqueous solution in the entry;
(2), the preparation isobutanol aluminum aqueous solution, with molar ratio computing, be 3 by the total amount of yttrium acetate and acetate europium in aqueous solution of preparation in (1), dry isobutanol aluminium amount is 5, take by weighing material after, be 1 with dry isobutanol aluminium again, water is 80～100 to take by weighing the water yield; Under 80-85 ℃ of temperature, dry isobutanol aluminium added then and make the aqueous solution in the entry;
(3), in contained yttrium acetate, acetate europium and isobutanol aluminum gross mass in the aqueous solution of (1) and (2) preparation, by 1 gram: 20cm
2The diode wafer ratio diode wafer of getting blue light-emitting or purple light put into reaction vessel and be fixed on reaction container bottom, then, the temperature that (1) is made is that 80-85 ℃ yttrium acetate, the acetate europium aqueous solution joins in the reaction vessel, keeping temperature is 80-85 ℃, the solution pH value is 4-6 and stirs the existence dropping isobutanol aluminum aqueous solution down, till the diode wafer surface forms gel, then diode wafer is taken out;
(4), the blue light-emitting of the surface attachment gel layer that takes out or the diode wafer of purple light are put into baking furnace, heating up in the dehydration back, forms europkium-activated yttrium-aluminium-garnet rete on 40 minutes top layers of 850 ℃ of-1100 ℃ of following sintering;
(5), with (4) make with the diode wafer of the europkium-activated yttrium-aluminium-garnet rete package lead again of cutting into slices according to a conventional method, be the white-light emitting diode finished product.
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| CNB200410018651XA CN1306628C (en) | 2004-01-30 | 2004-01-30 | Process for making white light diode by using blue light or purple light emitting diode chips |
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| CNB200410018651XA CN1306628C (en) | 2004-01-30 | 2004-01-30 | Process for making white light diode by using blue light or purple light emitting diode chips |
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| CN1306628C true CN1306628C (en) | 2007-03-21 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1364848A (en) * | 2001-09-18 | 2002-08-21 | 中国科学院长春光学精密机械与物理研究所 | Method for making luminous material glow with white light by purple light diode |
| JP2003332622A (en) * | 2002-05-13 | 2003-11-21 | Nikko Materials Co Ltd | Light emitting diode and its manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1364848A (en) * | 2001-09-18 | 2002-08-21 | 中国科学院长春光学精密机械与物理研究所 | Method for making luminous material glow with white light by purple light diode |
| JP2003332622A (en) * | 2002-05-13 | 2003-11-21 | Nikko Materials Co Ltd | Light emitting diode and its manufacturing method |
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