CN103497760A - Anti-phosphor deposition high thixotropic LED (light-emitting diode) jelly glue - Google Patents
Anti-phosphor deposition high thixotropic LED (light-emitting diode) jelly glue Download PDFInfo
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- CN103497760A CN103497760A CN201310430400.1A CN201310430400A CN103497760A CN 103497760 A CN103497760 A CN 103497760A CN 201310430400 A CN201310430400 A CN 201310430400A CN 103497760 A CN103497760 A CN 103497760A
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Abstract
The invention discloses anti-phosphor deposition high thixotropic LED (light-emitting diode) jelly glue. By selecting a coupling agent and optimizing hydrolysis conditions, a thixotropic material is obtained by modifying a gas phase, namely silicon dioxide, and anti-deposition phosphor is obtained by modifying phosphor. The thixotropic material is added into a silica gel system to obtain a high thixotropic silica gel system with a thixotropic index which is as high as 5; by adding different types and different contents of modified phosphor into the system, the jelly glue with different color temperatures can be integrally mixed, the jelly glue can not produce deposition within a shelf life of 3 months, and the color temperature value after packaging can be kept unchanged. The jelly glue disclosed by the invention is packaged by a needle cylinder, a mold is not required for assistance, the jelly glue can be directly fixed on a dispensing machine for use, and automatic forming is performed after dispensing. According to the jelly glue disclosed by the invention, the phosphor and the silica gel system are combined into a whole to prepare the jelly glue, the mold packaging step of an LED packaging link can be eliminated, the downstream packaging process is simplified, the production period is shortened, and the production efficiency is improved, so that the jelly glue has good application prospects.
Description
Technical field
The invention belongs to LED encapsulation technology field, particularly a kind of high thixotropic LED fruit juice gel of anti-fluorescent material sedimentation.
Background technology
As everyone knows, in the LED encapsulation, at first fluorescent material spot printing technique need fluorescent material and the silica gel bought are respectively mixed in proportion, the furnishing fluorescent glue.Fluorescent material is solia particle, and particle diameter is greatly between 7-25 μ m.Conventional two component addition silica gel viscosity are between 2000-6000cps.Because the fluorescent material particle diameter is excessive, silica gel viscosity is less than normal, cause fluorescent material to be easy to occur sedimentation in the silica gel system, usually within half an hour, finish using.If mixing time is long, fluorescent material generation sedimentation, can directly affect the consistence that LED encapsulates rear optics, i.e. colour temperature consistence and brightness uniformity etc.
In addition, along with the development of LED encapsulation technology, the continuous lifting of competitive power, shorten technique, enhancing productivity becomes the targets that great majority encapsulation producer is pursued.But generally the add-on type silica gel of use at high temperature all has mobility at present, want to make different rising angles, difform LED, must be by loaded down with trivial details mould process ability moulding when encapsulation, this shortens with the cycle that encapsulation producer is pursued undoubtedly, the target of cost is disagreed.In recent years, SHIN-ETSU HANTOTAI, DOW CORNING have released one after another and have had thixotropic single component silica gel, but its thixotropy index is not high, and automatic moulding is bad, and rising angle and light efficiency are all less than the effect of die package.Single-component additional organosilicon colloid ties up to that to add before thixotropic materials be Newtonian fuid, without thixotropy.After adding silicon-dioxide, its thixotropy is obviously improved, and along with the increase of add-on, it is large that thixotropy index becomes, and thixotropy improves, but that the negative impact brought is the agglomeration of silicon-dioxide is obvious, and the viscosity retrogradation, be unfavorable for operation.After photoelectricity test, transmittance descends, and the colloid mechanical property descends.Therefore, by adding the silicon-dioxide physical mixed to change its thixotropy, be impracticable.
For above-mentioned technological deficiency, for solving the settlement issues of fluorescent material in the silica gel system and realizing that LED is without the mould molding technology, the contriver develops efficient thixotropic materials, add the silica gel system can make high thixotropic silica gel, front end in encapsulation unites two into one modification fluorescent material and high thixotropic silica gel, make the high thixotropic phosphor gel of the anti-fluorescent material sedimentation of different-colour section, the contriver is by this phosphor gel called after fruit juice gel.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of high thixotropic LED fruit juice gel of anti-fluorescent material sedimentation is provided.
The technical solution used in the present invention is:
A kind of high thixotropic LED fruit juice gel of anti-fluorescent material sedimentation, for being mixed with the silica gel system of fluorescent material, contain aerosil in the silica gel system, and described fluorescent material and aerosil all adopt the silane coupling agent hydrolyzed solution to carry out modification.
Preferably, the preparation method of silane coupling agent hydrolyzed solution is as follows: mix methyl alcohol, water, glycerol, regulate pH to 2～4, then add silane coupling agent, stirring reaction 2～3h, obtain the silane coupling agent hydrolyzed solution; Wherein, in hydrolyzed solution, the concentration of glycerol is 2～4g/L.
Preferably, described silane coupling agent is at least one in KH570, KH560, KH171.
Preferably, in hydrolyzed solution, the volume fraction of methyl alcohol is 10～50%.
Preferably, in hydrolyzed solution, the volume fraction of silane coupling agent is 5～15%.
Preferably, the method for modifying of aerosil is as follows: gas mixture aerosil, organic solvent and silane coupling agent hydrolyzed solution, stir under 80～120 ℃, the 2～5h that refluxes, and remove organic solvent, dry, obtain; Wherein, the solubility of aerosil in organic solvent is 800～1200g/L.
Preferably, the weight ratio of aerosil and silane coupling agent hydrolyzed solution is 50～200:1.
Preferably, the method for modifying of fluorescent material is as follows: prepare the phosphor solution of 300～550g/L, after ultrasonic dispersion, add the silane coupling agent hydrolyzed solution, and stirring reaction 2～5h, washing, dry, and obtains.
Preferably, the weight ratio of fluorescent material and silane coupling agent hydrolyzed solution is 5～15:1.
Preferably, in the silica gel system, the content of modified gas aerosil is 2.5～4.0wt%.
The invention has the beneficial effects as follows:
(1) the present invention is by hydrolysising condition and the method for modifying of preferred coupling agent, optimization coupling agent, aerosil is carried out to modification, obtain thixotropic materials---modified gas aerosil, make this thixotropic materials under minimum add-on, the maximized thixotropic property that improves the silica gel system, in order to avoid add too much silicon-dioxide can affect light transmission and toughness and the operability of fruit juice gel.
(2) fluorescent material of the present invention, after silane coupler modified, embeds hydrophobic grouping at particle surface, it more easily is dispersed in high thixotropic silica gel system, and, due to dispersed raising, the brightness of fluorescent material also increases.
(3) the present invention is to the modification fluorescent material that adds different sorts, different content in high thixotropic silica gel system, the integrated fruit juice gel that mixes different-colour, this fruit juice gel is used within the longer quality guaranteed period (3 months), can not produce sedimentation, after encapsulation, color temperature value remains unchanged for a long time, has effectively solved common silica gel and has sneaked into the colour temperature offset issue that sedimentation causes after fluorescent material.
(4) fruit juice gel of the present invention has higher thixotropy index, and plasticity number is high, and product is the syringe packing, can directly be fixed on point gum machine and use, and does not need mould auxiliary, automatic moulding after some glue; Dimensional stabilizing after solidifying, do not shrink, indeformable, has consistent lighting angle.
(5) the present invention is to unite two into one to make fruit juice gel by fluorescent material and colloidal silica, can save the die package step of LED encapsulation link, has simplified the downstream packaging process, has reduced production cost, shortens the production cycle, has improved production efficiency.
The accompanying drawing explanation
The infrared spectrogram that Fig. 1 is unmodified fluorescent material YAG-04;
The infrared spectrogram that Fig. 2 is modification fluorescent material YAG-04;
The absorbance A that Fig. 3 is fruit juice gel 1# over time.
Embodiment
A kind of high thixotropic LED fruit juice gel of anti-fluorescent material sedimentation, for being mixed with the silica gel system of fluorescent material, contain aerosil in the silica gel system, and described fluorescent material and aerosil all adopt the silane coupling agent hydrolyzed solution to carry out modification.
Preferably, aerosil is hydrophobic silica.Preferably, the aerosil particle diameter is 7～14nm.Most preferred aerosil is watt gram H20, a H30.
Preferably, the preparation method of silane coupling agent hydrolyzed solution is as follows: mix methyl alcohol, water, glycerol, regulate pH to 2～4, then add silane coupling agent, stirring reaction 2～3h, obtain the silane coupling agent hydrolyzed solution; Wherein, in hydrolyzed solution, the concentration of glycerol is 2～4g/L.
Preferably, described silane coupling agent is at least one in KH570, KH560, KH171.
Preferably, in hydrolyzed solution, the volume fraction of methyl alcohol is 10～50%.
Preferably, in hydrolyzed solution, the volume fraction of silane coupling agent is 5～15%.
Preferably, the method for modifying of aerosil is as follows: gas mixture aerosil, organic solvent and silane coupling agent hydrolyzed solution, stir under 80～120 ℃, the 2～5h that refluxes, and remove toluene, dry, obtain; Wherein, the solubility of aerosil in organic solvent is 800～1200g/L.
Preferably, organic solvent is at least one in methyl alcohol, ethanol, toluene, benzene, dimethylbenzene.
Preferably, the weight ratio of aerosil and silane coupling agent hydrolyzed solution is 50～200:1.
Preferably, the method for modifying of fluorescent material is as follows: prepare the phosphor solution of 300～550g/L, after ultrasonic dispersion, add the silane coupling agent hydrolyzed solution, and stirring reaction 2～5h, washing, dry, and obtains.
Preferably, the weight ratio of fluorescent material and silane coupling agent hydrolyzed solution is 5～15:1.
Preferably, in the silica gel system, the content of modified gas aerosil is 2.5～4.0wt%.
Colloidal silica ties up to that to add before thixotropic materials be Newtonian fuid, and without thixotropy, after adding the thixotropic materials aerosil, thixotropy can obviously be improved.The research discovery, the quantity of aerosil surface hydroxyl can directly affect thixotroping effect and the mechanical property of silica gel system, and hydroxyl is more, and thixotropy is better, and tear strength is lower.The present invention selects suitable silane coupling agent to carry out modification to aerosil, makes its surrounding parcel silane, has effectively controlled the quantity of surface hydroxyl.Due to aerosil after the modification of coupling agent hydrolyzed solution, produce reactive force between hydrogen bond, Van der Waals force equimolecular between nano particle, the silica aggregate that these reactive forces make to be dispersed in system is connected to become a complete three-dimensional net structure, and be full of whole system, make the viscosity of system increase.When system is subject to shear action, hydrogen bond and Intermolecular Forces are destroyed, and the network of silica structure is also destroyed immediately, cause system viscosity to diminish; When shearing force disappears, network structure can be recovered again.Along with the increase of improved silica add-on, it is large that the thixotropy index becomes, and simultaneously, the viscosity of system is also increasing.
Consider the light transmission and toughness and the operability that add too much improved silica can affect fruit juice gel, the contriver optimizes the hydrolysising condition of coupling agent, and the mass ratio of hydrolyzed solution and aerosil, effectively controlled improved silica-OH content, make improved silica under minimum add-on, the maximized thixotropic property that improves the silica gel system.Fruit juice gel silica gel system thixotropy index of the present invention can be up to 5, utilize this performance can save the molding technique in the LED encapsulation, directly on point gum machine, operate, obtain the mould grain of semi-spherical shape, the diameter of mould grain and highly can determining according to air pressure, time and the syringe needle diameter of point gum machine.
Further, the mixture that fruit juice gel of the present invention is modification anti-settling fluorescent material and high thixotropic silica gel system.Fluorescent material, through silane coupler modified, embeds hydrophobic grouping at particle surface, on the one hand it more easily is dispersed in high thixotropic silica gel system, and, due to dispersed raising, the brightness of fluorescent material also increases.On the other hand; because the high thixotropic system is the non-Newtonian fluid type; the jelly colloid only just can flow when being subject to yielding stress; when static due to the existence of yield value; particle can stably be suspended in non-Newtonian fluid; therefore there is the effect of further anti-fluorescent material sedimentation; make fluorescent material settling velocity in system extremely slow; the gentle brightness of can not checking colors in longer validity period exerts an influence; effectively solved and joined the powder overlong time and cause sedimentation, thereby caused the drawback that colour temperature disunity, light splitting are unconcentrated.
The present invention, by changing kind and the proportion of fluorescent material, can be mixed with the fruit juice gel of different-colour value, and this fruit juice gel is single-component syringe packing.In the LED encapsulation process, substitute common mixed arogel water with fruit juice gel of the present invention, during encapsulation, only need definite colour temperature just can directly use the fruit juice gel of corresponding fluorescent material content to carry out a glue and subsequent job, not only save the mixed fluorescent material link in traditional technology, can also save loaded down with trivial details mould-forming process, greatly shorten life cycle of the product.
Modified gas aerosil of the present invention, modification fluorescent material can be mixed with the high thixotropic fruit juice gel that obtains anti-fluorescent material sedimentation with the conventional silica gel system of using in this area.
Below in conjunction with specific embodiment, further set forth content of the present invention.
The preparation technology of fruit juice gel is as follows:
(1) preparation of coupling agent KH560 hydrolyzed solution: get 5mL methyl alcohol and 45mL distilled water mixes, in this system, drip 0.1g(2g/L) glycerol, with acetic acid regulator solution pH=4, then add 5mL KH560, and the normal temperature lower magnetic force stirs 2h.Surveying its specific conductivity is 90 μ S/cm, proves that above method for hydrolysis can make coupling agent fully be hydrolyzed.
(2) processing of aerosil: get 100g watt of gram H30 in round-bottomed flask, the coupling agent hydrolyzed solution that adds 100 mL toluene and 1g step (1) to prepare, stirring, backflow 3h under 110 ℃.After having reacted, vacuum rotary steam is removed toluene, 60 ℃ of dried overnight in baking oven.
(3) modification aluminate fluorescent powder YAG-04(American I ntermatix company): take 7.8g YAG-04, add 15mL distilled water, ultrasonic dispersion 9min, obtain YAG-04 solution; Then be added dropwise to KH560 hydrolyzed solution prepared by 0.78g step (1), magnetic agitation 3h; Finally, use the separating funnel stratification, wash 3 times, dehydrated alcohol is washed (use absolute ethanol washing, easily dewater during oven dry, and fluorescent material is not easy to reunite) 2 times, in the baking oven of 60 ℃, dries, and obtains modification YAG-04.
(4) preparation of high thixotropic silica gel system: get respectively MQ resin 6000mPas 20g and 12000mPas 15g, get vinyl silicone oil 5000mPas 50g mixing as base glue.Add delayed-action activator acetylene hexalin 0.15g in base glue, fully, after mix and blend, add successively containing hydrogen silicone oil (hydrogen massfraction 0.8%) 2g and containing hydrogen silicone oil (hydrogen massfraction 0.42%) 3g to mix.Then add platinum water 0.1g, stir.The modification finally prepared by step (a 2) watt gram H30 2.5g joins in above system, and ultrasonic dispersion 20 minutes, obtain high thixotropic silica gel.
(5) preparation of fruit juice gel:
32.5g high thixotropic silica gel system prepared with step (4) by 2.6g modification fluorescent material YAG-04 prepared by step (3) is mixed (the proportion 8:100 of fluorescent material and silica gel), and ultrasonic dispersion, obtain fruit juice gel 1#.
embodiment 2
(1) preparation of coupling agent KH560 hydrolyzed solution: get 15mL methyl alcohol and 80mL distilled water mixes, in this system, drip the 0.3g glycerol, with acetic acid regulator solution pH=2, then add 5mL KH560, the normal temperature lower magnetic force stirs 3h.Surveying its specific conductivity is 88 μ S/cm, proves that above method for hydrolysis can make coupling agent fully be hydrolyzed.
(2) processing of aerosil: get 200g watt of gram H20 in round-bottomed flask, the KH560 hydrolyzed solution that adds 250mL methyl alcohol and 1g step (1) to prepare, stirring, backflow 2h under 120 ℃.After having reacted, vacuum rotary steam is removed methyl alcohol, 60 ℃ of dried overnight in baking oven.
(3) modification aluminate fluorescent powder YAG-04(American I ntermatix company): take 4.5g YAG-04, add 15mL distilled water, ultrasonic dispersion 9min, obtain YAG-04 solution; Then be added dropwise to KH560 hydrolyzed solution prepared by 0.3g step (1), magnetic agitation 2h; Finally, use the separating funnel stratification, wash 3 times, dehydrated alcohol is washed 2 times, in the baking oven of 60 ℃, dries, and obtains modification YAG-04.
(4) preparation of high thixotropic silica gel system: get respectively MQ resin 6000mPas 20g and 12000mPas 15g, get vinyl silicone oil 5000mPas 50g mixing as base glue.Add delayed-action activator 0.15g in base glue, fully, after mix and blend, add successively containing hydrogen silicone oil (hydrogen massfraction 0.8%) 2g and containing hydrogen silicone oil (hydrogen massfraction 0.42%) 3g to mix.Then add platinum water 0.1g, stir.The modification finally prepared by step (a 2) watt gram H20 3.8g joins in above system, and ultrasonic dispersion 20 minutes, obtain high thixotropic silica gel.
(5) preparation of fruit juice gel:
32.5g high thixotropic silica gel system prepared with step (4) by 3.25g modification fluorescent material YAG-04 prepared by step (3) is mixed (the proportion 10:100 of fluorescent material and silica gel), and ultrasonic dispersion, obtain fruit juice gel 2#.
embodiment 3
(1) preparation of coupling agent KH570 hydrolyzed solution: get 15mL methyl alcohol and 80mL distilled water mixes, in this system, drip the 0.3g glycerol, with acetic acid regulator solution pH=2, then add 5mL KH570, the normal temperature lower magnetic force stirs 3h.Surveying its specific conductivity is 85 μ S/cm, proves that above method for hydrolysis can make coupling agent fully be hydrolyzed.
(2) processing of aerosil: get 200g Cabot TS720 in round-bottomed flask, the KH570 hydrolyzed solution that adds 250mL dimethylbenzene and 1g step (1) to prepare, stirring, backflow 2h under 120 ℃.After having reacted, vacuum rotary steam is removed dimethylbenzene, 60 ℃ of dried overnight in baking oven.
(3) modification silicate fluorescent powder O5742(American I ntermatix company): take 4.5g O5742, add 15mL distilled water, ultrasonic dispersion 9min, obtain O5742 solution; Then be added dropwise to KH570 hydrolyzed solution prepared by 0.3g step (1), magnetic agitation 2h; Finally, use the separating funnel stratification, wash 3 times, dehydrated alcohol is washed 2 times, in the baking oven of 60 ℃, dries, and obtains modification O5742.
(4) preparation of high thixotropic silica gel system: get respectively MQ resin 6000mPas 20g and 12000mPas 15g, get vinyl silicone oil 5000mPas 50g mixing as base glue.Add delayed-action activator 0.15g in base glue, fully, after mix and blend, add successively containing hydrogen silicone oil (hydrogen massfraction 0.8%) 2g and containing hydrogen silicone oil (hydrogen massfraction 0.42%) 3g to mix.Then add platinum water 0.1g, stir.The modification Cabot TS720 2.8g finally prepared by step (2) joins in above system, and ultrasonic dispersion 20 minutes, obtain high thixotropic silica gel.
(5) preparation of fruit juice gel:
50g high thixotropic silica gel system prepared by 1.75g modification O5742 that in embodiment 2 prepared by 4.75g modification YAG-04, step (3) and step (4) is mixed, and ultrasonic dispersion, obtain fruit juice gel 3#.
embodiment 4
(1) preparation of coupling agent KH171 hydrolyzed solution: get 12mL methyl alcohol and 73mL distilled water mixes, in this system, drip the 0.4g glycerol, with acetic acid regulator solution pH=3, then add 15mL KH171, the normal temperature lower magnetic force stirs 3h.Surveying its specific conductivity is 83 μ S/cm, proves that above method for hydrolysis can make coupling agent fully be hydrolyzed.
(2) processing of aerosil: get 50g watt of gram H30 in round-bottomed flask, the KH171 hydrolyzed solution that adds 42mL benzene and 1g step (1) to prepare, stirring, backflow 5h under 80 ℃.After having reacted, vacuum rotary steam is removed benzene, 60 ℃ of dried overnight in baking oven.
(3) modification silicate fluorescent powder G2261(American I ntermatix company): take 6.0g G2261, add 15mL distilled water, ultrasonic dispersion 9min, obtain G2261 solution; Then be added dropwise to KH171 hydrolyzed solution prepared by 1.2g step (1), magnetic agitation 5h; Finally, use the separating funnel stratification, wash 3 times, dehydrated alcohol is washed 2 times, in the baking oven of 80 ℃, dries, and obtains modification G2261.
(4) preparation of high thixotropic silica gel system: get respectively MQ resin 6000mPas 20g and 12000mPas 15g, get vinyl silicone oil 5000mPas 50g mixing as base glue.Add delayed-action activator 0.15g in base glue, fully, after mix and blend, add successively containing hydrogen silicone oil (hydrogen massfraction 0.8%) 2g and containing hydrogen silicone oil (hydrogen massfraction 0.42%) 3g.Then add catalyzer 0.1g, stir.The modification finally prepared by step (a 2) watt gram H30 3.0g joins in above system, and ultrasonic dispersion 20 minutes, obtain high thixotropic silica gel.
(5) preparation of fruit juice gel:
50g high thixotropic silica gel system prepared by 5g modification G2261 that in embodiment 3 prepared by 3g modification O5742, step (3) and step (4) is mixed, and obtains fruit juice gel 4#.
embodiment 5
By selecting the aerosil (in Table 1) of different brands, different-grain diameter, respectively it is carried out to surface modification treatment according to the described method of embodiment 1 step (2), obtain thixotropic materials (modified gas aerosil); Then, according to the described method of embodiment 1 step (4), make respectively different high thixotropic silica gel.
Performance test:
The test of A, thixotropy: with the viscosity of HBDV-II viscosmeter 52# rotor measurement high thixotropic silica gel, thixotropy characterizes with thixotropy index, refers to record at 0.5 r/min the ratio that viscosity and 5.0 r/min record viscosity.
B, transmittance test: LS102 optical transmittance survey meter, wavelength is 450nm, silica gel piece thickness is 1mm.
Test result is in Table 1.
Performance perameter after the different aerosil modifications of table 1
| Model | Cabot TS720 | Degussa A200 | Degussa R974 | Degussa R812S | Watt gram H20 | Watt gram H30 | Watt gram T40 |
| Type | Hydrophobic | Hydrophilic | Hydrophobic | Hydrophobic | Hydrophobic | Hydrophobic | Hydrophilic |
| Particle diameter (nm) | 13 | 12 | 12 | 7 | 14 | 9 | 7 |
| Content (wt%) | 3.4 | 3.4 | 3.4 | 3.4 | 3.4 | 3.4 | 3.4 |
| Thixotropy index | 3 | 1.2 | 2 | 2.3 | 3.8 | 4 | 1.4 |
| (450nm, 1mm is thick, %) for transmittance | 88 | 95 | 89 | 92 | 92 | 91 | 94 |
| Tear strength (MPa) | 5 | 3 | 4 | 4.5 | 6 | 6.2 | 5 |
By the analysis of his-and-hers watches 1 data, in the improved silica of same amount, the best results of watt gram H30, when its add-on is 4%, thixotropy index is up to 5, transmittance 88%, tear strength 7.0MPa.
embodiment 6
Prove by simultaneous test the character that thixotropic materials and modification fluorescent material possess in fruit juice gel.
(1) preparation of fruit juice gel
Fruit juice gel a: unmodified YAG-04 is substituted to modification YAG-04, and other components and preparation method are with fruit juice gel 1#.
Fruit juice gel b: unmodified watt of gram H30 substituted to modification watt gram H30, and other components and preparation method are with fruit juice gel 1#.
Performance test:
A, fluorescent material is carried out to Infrared spectroscopy
Result is (Fig. 1,2 is respectively the infrared spectrogram of the YAG-04 after unmodified and modification) as shown in Figure 1 and Figure 2, visible, and the fluorescent material after modification is at 1022.27cm
-1new absorption peak appears in place, is attributed to the stretching vibration absorption peak of C-O singly-bound, modification is described after fluorescent material contain epoxy group(ing), that is, prove between YAG-04 and coupling agent A187 bonding action occurred.
The change in concentration (chemical process) of B, test fruit juice gel 1#
Testing apparatus: Agilent HP-8453
Test philosophy: with ultraviolet, visible light light-splitting photometer, measure in 5 minutes cuvettes certain any fruit juice gel absorbancy (A).According to Beer-Lambert law, the variation of A and concentration (C) be varied to direct ratio, thereby detect within for some time certain any concentration, whether change.
Test condition:
1) certain in cuvette is a bit tried one's best near the upper surface of fruit juice gel, if sedimentation occurs, fluorescent material is from topmost starting to sink, so topmost the fluorescent material concentration of any is that in whole cuvette, change is the most obvious;
2) other position of cuvette is wrapped by lighttight black paper bag;
3) 10 points are got in on-line testing altogether, and the whole test duration is 45 minutes;
4) get the test data under the maximum absorption wavelength 558nm of YAG-04.
Test result as shown in Figure 3, can find out, the value of absorbance A slightly descended in 45 minutes, but fall is very little.The concentration value of being calculated by Beer-Lambert equation changes very little, in the scope of error, can ignore.Illustrate that in this time period, sedimentation occurs fluorescent material hardly.
The color temperature value of C, test fruit juice gel is (photoelectric method) over time
Whether common silica gel has sedimentation after sneaking into fluorescent material, and concentration can from top to bottom become greatly gradually, therefore only need investigate the color temperature value of syringe different heights place fruit juice gel, with regard to provable fluorescent material concentration in the silica gel system, change, and whether produces sedimentation.
Test procedure:
1) get fruit juice gel 1#, each 30g of fruit juice gel a, pack with the 30cc syringe respectively, vertically be placed on 4 ℃ of refrigerator and cooled and hide 2 months.
2) take out under the syringe room temperature and rise again 2 hours, make a glue and have the pattern grain of one's own on the COB substrate, do 5 mould grains at every turn while getting glue.Mould grain quality is all in limit of error, and the weight in average of single mould grain is 0.007g.
3) photoelectricity test: during without the fluorescent material sedimentation, reference color temperature should be at 6000 ± 200(k).
Test result is in Table 2,3.
The color temperature value contrast of table 2 fruit juice gel 1#, a point glue after the different positions sampling of syringe
The color temperature value contrast of table 3 fruit juice gel 1#, b point glue after the different positions sampling of syringe
By the analysis of table 2,3 data, in the different zones of syringe, the color temperature value of fruit juice gel 1# mainly concentrates in 6000 ± 100k scope, and light splitting is concentrated, and illustrates that fluorescent material is without obvious sedimentation, places after 3 months and does not affect the photoelectricity colour temperature.And the color temperature value scope of fruit juice gel a has exceeded the standard range of colour temperature at 6000 ± 300k, illustrate that the sedimentation of fluorescent material is apparent in view, the colour temperature fluctuation is larger.The color temperature value scope of fruit juice gel b, at 6000 ± 300k, concentrates color temperature value at 6000 ± 200k, wider than the color temperature distribution of fruit juice gel 1#, narrower than the color temperature distribution of fruit juice gel a.Illustrate that modification fluorescent material and modified gas aerosil have contribution to the consistence of color temperature value.
Above two kinds of methods of surveying the fluorescent material sedimentation have all well proved that the fluorescent material after the modification can not produce sedimentation in high thixotroping silica gel system, in storage period (according to the photoelectricity test result, the shelf lives is 3 months), can not affect the size of color temperature value.
Apply above-mentioned photoelectric method test fruit juice gel 2#～4# color temperature value over time, result also proves that its color temperature value is stable in 3 months shelf lifes.
embodiment 7
formulate the fruit juice gel of different-colour:
By add the modification fluorescent material of different sorts, different content in high thixotropic silica gel system, integration system is made the high thixotropic fruit juice gel product of the anti-fluorescent material sedimentation of different-colour size.
The contriver is by determining photoelectric parameter, the mould grain size parameter of the encapsulation of COB flip-chip mould grain, determines the proportion of fluorescent material and silica gel system in embodiment 1 ~ 4, drawn color temperature value and the colour rendering index of correspondence with it, in Table 4,5.
Photoelectric parameter and the mould grain parameter of the encapsulation of table 4 COB flip-chip mould grain
The corresponding relation of table 5 arogel proportion and color temperature value
| The fruit juice gel numbering | The fluorescent material type | Arogel proportion | Colour temperature (k) | |
| 1# | Bloom | 8：100 | 6500±200 | 75 |
| 2# | Bloom | 10：100 | 5200±200 | 70 |
| 3# | Bloom+rouge and powder | 13：100 | 4200±200 | 70 |
| 4# | Yellowish green powder+rouge and powder | 16：100 | 3000±200 | 65 |
1) annotate: the proportion that arogel proportion is fluorescent material and silica gel system.
Certainly, the fruit juice gel of allotment different-colour value is not limited to above-described embodiment, to the change of arbitrary parameter wherein, all can obtain different reference color temperatures.
Claims (10)
1. the high thixotropic LED fruit juice gel of an anti-fluorescent material sedimentation, for being mixed with the silica gel system of fluorescent material, contain aerosil in the silica gel system, and described fluorescent material and aerosil all adopt the silane coupling agent hydrolyzed solution to carry out modification.
2. fruit juice gel according to claim 1, it is characterized in that: the preparation method of silane coupling agent hydrolyzed solution is as follows: mix methyl alcohol, water, glycerol, regulate pH to 2～4, then add silane coupling agent, stirring reaction 2～3h, obtain the silane coupling agent hydrolyzed solution; Wherein, in hydrolyzed solution, the concentration of glycerol is 2～4g/L.
3. fruit juice gel according to claim 2, it is characterized in that: described silane coupling agent is at least one in KH570, KH560, KH171.
4. fruit juice gel according to claim 2, it is characterized in that: in hydrolyzed solution, the volume fraction of methyl alcohol is 10～50%.
5. fruit juice gel according to claim 2, it is characterized in that: in hydrolyzed solution, the volume fraction of silane coupling agent is 5～15%.
6. according to the described fruit juice gel of claim 1～5 any one, it is characterized in that: the method for modifying of aerosil is as follows: gas mixture aerosil, organic solvent and silane coupling agent hydrolyzed solution, stir under 80～120 ℃, the 2～5h that refluxes, and remove organic solvent, dry, obtain; Wherein, the solubility of aerosil in organic solvent is 800～1200g/L.
7. fruit juice gel according to claim 6, it is characterized in that: the weight ratio of aerosil and silane coupling agent hydrolyzed solution is 50～200:1.
8. according to the described fruit juice gel of claim 1～5 any one, it is characterized in that: the method for modifying of fluorescent material is as follows: prepare the phosphor solution of 300～550g/L, after ultrasonic dispersion, add the silane coupling agent hydrolyzed solution, stirring reaction 2～5h, washing, dry, obtain.
9. fruit juice gel according to claim 8, it is characterized in that: the weight ratio of fluorescent material and silane coupling agent hydrolyzed solution is 5～15:1.
10. fruit juice gel according to claim 1, it is characterized in that: in the silica gel system, the content of modified gas aerosil is 2.5～4.0wt%.
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| CN115197690A (en) * | 2022-07-13 | 2022-10-18 | 江门市科恒实业股份有限公司 | Orange-red fluorescent powder and preparation method thereof |
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