CN103562290A - Thermosetting resin composition for light reflection, preparation method thereof, reflecting plate for loading photonic semiconductor prepared therefrom, and photonic semiconductor device containing same - Google Patents
Thermosetting resin composition for light reflection, preparation method thereof, reflecting plate for loading photonic semiconductor prepared therefrom, and photonic semiconductor device containing same Download PDFInfo
- Publication number
- CN103562290A CN103562290A CN201280024015.0A CN201280024015A CN103562290A CN 103562290 A CN103562290 A CN 103562290A CN 201280024015 A CN201280024015 A CN 201280024015A CN 103562290 A CN103562290 A CN 103562290A
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- China
- Prior art keywords
- luminous reflectance
- heat curing
- type luminous
- resin combination
- resin
- Prior art date
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920001187 thermosetting polymer Polymers 0.000 title abstract description 5
- 239000011342 resin composition Substances 0.000 title abstract 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims description 68
- 229920005989 resin Polymers 0.000 claims description 67
- 239000011347 resin Substances 0.000 claims description 67
- 239000003795 chemical substances by application Substances 0.000 claims description 53
- 239000003822 epoxy resin Substances 0.000 claims description 41
- 229920000647 polyepoxide Polymers 0.000 claims description 41
- 239000003054 catalyst Substances 0.000 claims description 37
- 239000011256 inorganic filler Substances 0.000 claims description 35
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 35
- 230000003287 optical effect Effects 0.000 claims description 32
- 238000007669 thermal treatment Methods 0.000 claims description 22
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- 239000000126 substance Substances 0.000 claims description 18
- 238000012360 testing method Methods 0.000 claims description 16
- 230000000996 additive effect Effects 0.000 claims description 15
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- 238000002844 melting Methods 0.000 claims description 14
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- 238000001879 gelation Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 125000004432 carbon atom Chemical group C* 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
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- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 4
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- MNAHQWDCXOHBHK-UHFFFAOYSA-N 1-phenylpropane-1,1-diol Chemical compound CCC(O)(O)C1=CC=CC=C1 MNAHQWDCXOHBHK-UHFFFAOYSA-N 0.000 description 2
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 2
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- 239000006087 Silane Coupling Agent Substances 0.000 description 2
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- 150000001336 alkenes Chemical class 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 239000004305 biphenyl Substances 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
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- 239000011353 cycloaliphatic epoxy resin Substances 0.000 description 2
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 230000032050 esterification Effects 0.000 description 2
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- UTOPWMOLSKOLTQ-UHFFFAOYSA-N octacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O UTOPWMOLSKOLTQ-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
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- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
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- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 description 1
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- BLBVJHVRECUXKP-UHFFFAOYSA-N 2,3-dimethoxy-1,4-dimethylbenzene Chemical compound COC1=C(C)C=CC(C)=C1OC BLBVJHVRECUXKP-UHFFFAOYSA-N 0.000 description 1
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- 150000004756 silanes Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- RINCXYDBBGOEEQ-UHFFFAOYSA-N succinic anhydride Chemical compound O=C1CCC(=O)O1 RINCXYDBBGOEEQ-UHFFFAOYSA-N 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Chemical group 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/58—Optical field-shaping elements
- H01L33/60—Reflective elements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/62—Alcohols or phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0025—Crosslinking or vulcanising agents; including accelerators
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/62—Arrangements for conducting electric current to or from the semiconductor body, e.g. lead-frames, wire-bonds or solder balls
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Epoxy Resins (AREA)
Abstract
The present invention relates to a thermosetting resin composition for light reflection, a preparation method thereof, a reflecting plate for loading a photonic semiconductor prepared therefrom, and a photonic semiconductor device containing the same. More specifically, the present invention relates to a thermosetting resin composition for light reflection, a preparation method thereof, a reflecting plate for loading a photonic semiconductor prepared therefrom, and a photonic semiconductor device containing the same. The thermosetting resin composition for light reflection comprises a polyol containing two or more hydroxyl groups as a curing accelerator, has excellent discoloration resistance, does not become yellow or discolor, and cause less reduction of light reflectance.
Description
Technical field
The present invention relates to a kind of heat curing-type resin combination and preparation method thereof for luminous reflectance, utilize optical semiconductor prepared by described composition carry with reflector and comprise that described optical semiconductor carries the optical semiconductor device of use reflector.More specifically, the present invention relates to resin combination and preparation method thereof for a kind of heat curing-type luminous reflectance, utilize optical semiconductor prepared by described composition carry with reflector and comprise that described optical semiconductor carries the optical semiconductor device with reflector, wherein said heat curing-type luminous reflectance with resin combination comprise there are 2 above hydroxyls polyvalent alcohol as curing catalyst, there is excellent anti-discoloration, therefore can xanthochromia or variable color, and less reduce luminous reflectance factor.
Background technology
LED (light emitting diode) is element mounted on reflector, and the light-emitting device sealing with epoxy resin etc.Therefore such LED is less, lighter, be easily loaded in various devices, and shake or ON/OFF (on/off) repeatedly owing to resist, so it is long to have the life-span, bright-colored and obvious and have advantages of that identity, energy consumption are low.In this type of LED, the White LED of the fluor of white light is sent in ultraviolet ray emitting element and the ultraviolet ray being produced by described ultraviolet ray emitting element, as at background lights of liquid crystal display such as mobile phone, computer, TVs, the light source of the headlight of automobile or dashboard, illuminating device etc. enjoys attracting attention of people.
The LED reflector using on this kind of device, the light that conventionally need to be able to send luminous element or ultraviolet high-efficiency reflective, good luminous reflectance factor.Low in order to prevent luminous reflectance factor, should avoid reflector itself xanthochromia or variable color can not occur.And because LED reflector long-term exposure is in high temperature, so it need to also should have higher luminous reflectance factor after thermal treatment.
Existing LED reflector is first from tinsel, by known methods such as punching press or etchings, to form metal winding displacement, then on metal winding displacement (lead frame), carries out with comprising the thermoplastic resin molded of white pigment, making after nickel plating/metals such as silver.But due to the demand of human consumer for high brightness, the rated output of nearest LED is higher.The high temperature and the ultraviolet ray that now produce make the variable colors such as reflector generation xanthochromia, become and cause the major cause that luminous reflectance factor reduces and brightness reduces.The existing luminous reflectance reflector of manufacturing with thermoplastic resin finished product, it is limited particularly at high temperature maintaining luminous reflectance factor.
Summary of the invention
The technical problem solving
The object of the invention is to, a kind of do not occur xanthochromia or variable color are provided, the heat curing-type luminous reflectance resin combination that anti-discoloration is outstanding.
Another object of the present invention is to, provide a kind of after thermal treatment, luminous reflectance factor does not reduce, and heat curing-type luminous reflectance resin combination that can transfer molding.
Another object of the present invention is, the preparation method of a kind of heat curing-type luminous reflectance with resin combination is provided.
Another object of the present invention is, a kind of optical semiconductor lift-launch reflector is provided, and it comprises: the reflector forming with resin combination with described heat curing-type luminous reflectance.
Another object of the present invention is, a kind of optical semiconductor device is provided, and it comprises: described mounting semiconductor element reflector.
Technical scheme
Heat curing-type luminous reflectance resin combination according to an aspect of the present invention, its comprise there are 2 above hydroxyls polyvalent alcohol as curing catalyst, the sustainment rate of the luminous reflectance factor being represented by following formula 1 of the test piece of being prepared by described composition can reach approximately more than 70%.
< formula 1>
Luminous reflectance factor * 100 before the luminous reflectance factor/thermal treatment of the sustainment rate of luminous reflectance factor (%)=180 ℃ of thermal treatments after approximately 168 hours
In one concrete example, described composition, after transfer molding, solidifies approximately 3 hours at 150 ℃, then the sustainment rate of the luminous reflectance factor after 168 hours can reach approximately more than 70% 180 ℃ of thermal treatments.
In one concrete example, described composition when transfer molding, helicoidal flow length (Spiral Flow Length(S/F)) be about 15-45 inch.
In one concrete example, described composition when transfer molding, gelation time (gelation time(G/T)) be about 30-70 second.
In one concrete example, described composition can comprise: described curing catalyst, epoxy resin, solidifying agent, inorganic filler and white pigment.
In one concrete example, described curing catalyst can have the structure of following chemical formula 3.
< chemical formula 3>
OH-(CH
2)
m-[CR
1-OH]
n-(CH
2)
p-OH
(in described formula, R
1line style or the ramiform alkyl of hydrogen or carbonatoms 1-30; N is the integer of 0-20; M and p are independently the integers of 0-10.But n, m and p are except 0 situation entirely)
In one concrete example, described curing catalyst can not comprise aromatic group.
In one concrete example, described curing catalyst, with respect to the epoxy resin of 100 weight parts, can comprise about 3-49 weight part.
In one concrete example, described epoxy resin can not comprise aromatic group.
In one concrete example, described solidifying agent can not comprise aromatic group.
In one concrete example, described composition also can comprise: the more than one material of selecting in the group being comprised of releasing agent and additive.
In one concrete example, described inorganic filler can comprise: the inorganic filler of the not enough approximately 10 μ m of median size (D50) and the mixture that median size (D50) is about the inorganic filler of 10-35 μ m.
In one concrete example, described in described composition, the ratio of white pigment and inorganic filler is about 1:0.1 to 1:4 weight ratio.
The preparation method of resin combination for heat curing-type luminous reflectance according to a further aspect of the invention, comprising: by epoxy resin and solidifying agent melting mixing; And in described mixture, curing catalyst, inorganic filler and the white pigment that interpolation comprises the polyvalent alcohol with approximately 2 above hydroxyls is with the step of melting mixing.
In one concrete example, described melting mixing step can be at the temperature of about 30-50 ℃, carries out approximately 30 to 180 minutes.
Optical semiconductor lift-launch reflector according to another aspect of the invention, can comprise described heat curing-type luminous reflectance resin combination.
Optical semiconductor device according to another aspect of the invention, can comprise described optical semiconductor lift-launch reflector.
Beneficial effect
The invention provides a kind of excellent anti-discoloration that has, therefore the heat curing-type luminous reflectance resin combination of flavescence or variable color can not occur.In addition, the invention provides a kind ofly under being exposed to for a long time high temperature time, the reflective heat curing-type luminous reflectance resin combination of penetrating the reduction of rate can not occur yet.
Accompanying drawing explanation
Fig. 1 is sample prepared by the composition of the composition of embodiment 1-3 and comparative example 4,180 ℃ of thermal treatments after approximately 168 hours, under 430nm wavelength, the variation of the luminous reflectance factor changing with digestion time (aging time), wherein the composition of embodiment 4 contains the curing catalyst with aromatic group.
Fig. 2 is sample prepared by the composition of the composition of embodiment of the present invention 1-3 and comparative example 5-7,180 ℃ of thermal treatments after approximately 168 hours, under 430nm wavelength, the variation of the luminous reflectance factor changing with digestion time, wherein the composition of comparative example 5-7 contains the thermoplastic resin in the past using.
Embodiment
The sustainment rate of the luminous reflectance factor of the resin combination that heat curing-type luminous reflectance is according to an aspect of the present invention used can reach approximately more than 70%.In this specification sheets, " sustainment rate of luminous reflectance factor " of indication refers to the test piece of being prepared by described resin combination, and the luminous reflectance factor 180 ℃ of thermal treatments after approximately 168 hours, with respect to the ratio of the luminous reflectance factor before thermal treatment.The sustainment rate of luminous reflectance factor can represent according to following formula 1.
< formula 1>
Luminous reflectance factor * 100 before the luminous reflectance factor/thermal treatment of the sustainment rate of luminous reflectance factor (%)=180 ℃ of thermal treatments after approximately 168 hours
Conventionally, when the test piece of being prepared with resin combination by luminous reflectance is heat-treated, its color can be from white yellowing, and it is to reduce caused because of luminous reflectance factor.Luminous reflectance factor reduces less, and its anti-discoloration is higher.The sustainment rate that is luminous reflectance factor is higher, and anti-discoloration is just higher.
The sustainment rate of the luminous reflectance factor of described composition can reach approximately more than 70%, preferably, can reach about 72-85%.
Although the sustainment rate to described luminous reflectance factor is not particularly limited, can utilize transfer molding machine, composition, the temperature compacted under of 150 ℃ 240 seconds, from mould takes off, then is carried out to the after fixing of 3 hours the temperature of 150 ℃, thus preparation test piece.Afterwards, detect the luminous reflectance factor before thermal treatment, and at 180 ℃ of temperature, carry out detecting luminous reflectance factor after the thermal treatment of 168 hours, and through further calculating and drawing.In the present invention, described luminous reflectance factor is that to take the value detecting under 430nm wavelength be benchmark.
In one concrete example, described heat curing-type luminous reflectance is with resin combination when transfer molding, and its helicoidal flow length is about 15-45 inch.Preferably, can be about 24-45 inch.
In one concrete example, the resin combination that described heat curing-type luminous reflectance is used when transfer molding, its gelation time (gelation time(G/T)) can be about 30-70 second, preferably, can be about 57-68 second.
Resin combination of the present invention can comprise: epoxy resin, solidifying agent, curing catalyst, inorganic filler and white pigment.
In the present invention, epoxy resin can be used conventional epoxy resin molding material.Specifically have: the resol of Pyrogentisinic Acid's class and aldehydes carries out epoxidised resin, comprise phenol phenol aldehyde type epoxy resin, Study On O-cresol Epoxy Resin etc.; Diglycidyl ether, comprises that dihydroxyphenyl propane, Bisphenol F, bisphenol S and hydrocarbon are for bis-phenol etc.; The glycidyl amine type epoxy resin being obtained by the reaction of the polyamine such as diaminodiphenylmethane, isocyanuric acid and epoxy chloropropionate alcohol; The line style aliphatic epoxy resin that alkene key is obtained with peracid moulding such as high acetic acid; And cycloaliphatic epoxy resin etc.Epoxy resin also can mix two or more use.
Epoxy resin is the resin that epoxy equivalent (weight) is about 50-500g/eq.Preferably, can use the epoxy resin that is about 80-450g/eq.
Preferably, can use the epoxy resin that does not comprise aromatic group.Comprise aromatic group, and while being applied to the reflector of luminous element, can produce xanthochromia because of the high temperature of luminous element, cause using as reflector.For example, epoxy resin can be used the line style aliphatic epoxy resin that alkene key is obtained with peracid moulding such as high acetic acid; And cycloaliphatic epoxy resin etc.
For example, in epoxy resin, also can use the triglycidyl isocyanurate resin of following Chemical formula 1 of the transparency and anti-discoloration excellence or the epoxy resin of following Chemical formula 2.
< Chemical formula 1 >
< Chemical formula 2 >
(said n is the integer of 0-20)
Especially, because the epoxy resin of described formula 2 is to comprise approximately more than one hydroxyl in epoxy molecular structure, therefore be relatively applicable to being prepared into the B stage (B stage) of thermosetting resin, it can be because react gelation occurs with the partial esterification of solidifying agent, and can again be melted after heating.
The compound that can react with described epoxy resin for the solidifying agent that can use in the present invention, is not particularly limited, so long as all can be used.Solidifying agent can be used anhydride curing agent, isocyanuric acid solidifying agent, phenol solidifying agent etc.Solidifying agent can mix two or more use.
Anhydride curing agent can be used Tetra hydro Phthalic anhydride, MALEIC ANHYDRIDE, trimellitic acid 1,2-anhydride, PMA, hexahydrophthalic anhydride, Tetra Hydro Phthalic Anhydride, methyl carbic anhydride, carbic anhydride, Pyroglutaric acid, dimethylated pentanedioic acid acid anhydride, diethyl glutarate acid anhydride, succinyl oxide, methylhexahydrophthalic anhydride and methyl tetrahydrophthalic anhydride etc.
Isocyanuric acid solidifying agent comprises: 1,3,5-tri-(1-carboxymethyl) isocyanuric acid ester, 1,3,5-tri-(2-carboxymethyl) isocyanic ester, 1,3,5-tri-(3-carboxymethyl) isocyanuric acid ester, 1, two (2-carboxymethyl) isocyanuric acid esters of 3-etc.
Phenol solidifying agent can be used the compound aphthols of the phenol such as phenol, cresols, Resorcinol, pyrocatechol, dihydroxyphenyl propane, Bisphenol F, phenylphenol, amino phenol and/or naphthyl alcohol, 2-Naphthol, dihydroxy naphthalene etc. and formaldehyde, phenyl aldehyde, salicylic aldehyde etc. to aldehyde radical, polymerization or cocondensation under the condition of an acidic catalyst and the novolac type phenolic resin that obtains; By phenol and/or aphthols and dimethoxy p-Xylol or the synthetic phenol-aralkyl resin of two (methoxyl group) biphenyl; The aralkyl-type phenolic resins such as biphenyl type phenol-aralkyl resin, naphthols-aralkyl resin; The dicyclopentadiene-type phenolic resin such as synthetic dicyclopentadiene-type phenol resol, dicyclopentadiene-type naphthol novolac resin by the copolymerization of phenols and/or aphthols and Dicyclopentadiene (DCPD); Tritane type phenolic resin; Modification terpene phenol resin; Modification p-Xylol and/or m-xylene phenolic resin; Modified cyanurotriamide phenolic resin; Or modification cyclopentadiene phenolic resin.
Preferably, can use the solidifying agent that does not comprise aromatic group.
Comprise aromatic group, and while being applied to the reflector of photodiode, because the high temperature of photodiode produces xanthochromia, make cannot use as reflector.For example, in the group that can be formed by anhydride curing agent and isocyanuric acid solidifying agent, select at least one, as solidifying agent.Preferably, can use anhydride curing agent.
Anhydride curing agent be take and used colourless or flaxen solidifying agent as good.
Solidifying agent, with respect to the described epoxy resin of 100 weight parts, can comprise about 50-250 weight part.In described scope, can have that high-temperature stability and excellent electric property, thermal change type temperature are high, the effect of good mechanical property.Preferably, about 50-200 weight part can be comprised, more preferably, about 50-170 weight part can be comprised.
For the solidifying agent of epoxy resin, especially, with the proportioning of anhydride curing agent, for the epoxide group in the epoxy resin of 1 equivalent, preferably use the active group that can react with epoxide group of about 0.5-1.5 equivalent, for example anhydride group.In described scope, the glass tansition temperature of the solidification rate of composition epoxy resin, cured article and the wet fastness of cured article all can not reduce.Preferably, can use about 0.7-1.2 equivalent.
Except the solidifying agent for described epoxy resin, also can together use with alcohol the solidifying agent of described anhydride curing agent partial esterification or carboxylic acid solidifying agent.
Spendable curing catalyst can react with described epoxy resin and solidifying agent in the present invention, thereby plays the effect that promotes crosslinking reaction.Curing catalyst can be used the polyvalent alcohol with approximately 2 above hydroxyls.Preferably, curing catalyst can have approximately 3 above hydroxyls.
For curing catalyst, there is no special restriction, it can have the structure of following chemical formula 3.
< chemical formula 3>
OH-(CH
2)
m-[CR
1-OH]
n-(CH
2)
p-OH
(in above-mentioned formula, R
1hydrogen or the line style of carbonatoms 1-30 or the alkyl of ramiform; N is the integer of 0-20; M and p are independently the integers of 0-10.But n, m and p are except 0 situation entirely)
Preferably, R1 is hydrogen or the line style of carbonatoms 1-10 or the alkyl of ramiform; N is the integer of 0-3.
Curing catalyst of the present invention can be used hydroxyl equivalent to be about more than 30; Preferably be about 30-200; More preferably, be about 30-150 curing catalyst.
Curing catalyst of the present invention can not comprise aromatic group.As comprise aromatic group, while preparing reflector, may there is variable color.
Curing catalyst of the present invention, with respect to the described epoxy resin of 100 weight parts, can comprise about 3-49 weight part.In described scope, because epoxy resin and solidifying agent are not cross-linked, can prevent the state that composition is uncured.Preferably, can comprise about 5-45 weight part.
To inorganic filler, there is no particular limitation.For example, can use and in the group being formed by silicon-dioxide, aluminium hydroxide, magnesium hydroxide, barium sulfate, magnesiumcarbonate, barium carbonate, select at least one above inorganic filler.From formability and the flame retardant resistance of resin combination, consider, preferably use electrodeless weighting agent more than at least one that select from silicon-dioxide, aluminium hydroxide and magnesium hydroxide.
The median size of inorganic filler (D50) is below approximately 35 μ m, preferably, can be about 1-22 μ m.Inorganic filler also can mix the mutual different inorganic filler of median size of more than two kinds to be used.For example, median size (D50) can be about below 10 μ m, the inorganic filler that to be preferably about the inorganic filler of 1-9.99 μ m and median size (D50) be about 10-35 μ m mixes and uses.Comprise when median size (D50) is about the inorganic filler of 10-35 μ m, when transfer molding, can thering is the effect that reduces the overlap (flash) producing between mould.If but too much time, easily stopped up the inlet of noting chamber, the situation of fully not filling would be caused.The inorganic filler that now, can comprise the not enough approximately 10 μ m of median size (D50): the weight ratio that median size (D50) is about the inorganic filler of 10-35 μ m is about 1:0.1 to the inorganic filler of about 1:20.
With respect to heat curing-type luminous reflectance, with in total 100 weight parts of resin combination, inorganic filler can be used about 1-90 weight part.Preferably, be about 5-70 weight part, more preferably, be about 40-45 weight part.
For white pigment, be not particularly limited, can use titanium oxide, aluminum oxide, magnesium oxide, weisspiessglanz, zirconium white and inorganic hollow particle.
The median size of white pigment (D50) is about 0.1 to 50 μ m.In described scope, because particle does not condense, therefore, its good dispersity, and the reflective character of cured article can variation.
White pigment can mix the different white pigment of more than two kinds of use median size.
Total 100 weight parts of the resin combination of using with respect to heat curing-type luminous reflectance, white pigment can be used about 5-50 weight part, preferred about 10-40 weight part, more preferably from about 15-35 weight part.
For white pigment and inorganic filler, white pigment: the weight ratio of inorganic filler is about the weight ratio of 1:0.1 to 1:4.In described scope, the reflective character of cured article can variation, and be conducive to flat board (tablet) moulding for transfer molding method, when injecting solute in mould, can reduce the generation that the foam of obstruction luminous reflectance occurs finished surface, also can reduce the resin burr from overflowing between mould, do not produce the pollution of the metal winding displacement (lead frame) being caused by resin burr, when optical semiconductor is equipped on to metal winding displacement, there is good welding operation and be connected the effect of operation with metal wire.The weight ratio that preferably, can comprise about 1:0.2 to 1:3.
In another concrete example, composition of the present invention also can comprise more than one the material of selecting in the group being comprised of releasing agent and additive.
For releasing agent, have no particular limits, can have in the group that the oxidized form polyolefine of carboxyl forms and select at least one above use by aliphatic carboxylic acid, aliphatic carboxylic acid esters,, aliphatic polyether, Non-oxidized Polyolefin and.Preferably, use colourless or flaxen painted more shallow releasing agent.
Aliphatic carboxylic acid, can be used the monobasic organic acid that the carbonatomss such as lauric acid, myristic acid, palmitinic acid, stearic acid and montanic acid are 10-50.
Aliphatic carboxylic acid esters,, can use polyalkylene ether (polyakylene ether) compound of the carbonatoms 3-500 with following chemical formula 4 structures.
< chemical formula 4>
(above-mentioned q1 is 1-20, and R is the organic group of hydrogen, methyl, carbonatoms 2-10)
The polyolefine of oxidized form or Non-oxidized, can be used number-average molecular weight to be about the low-molecular-weight polyolefin of 500-10000g/mol.
For the epoxy resin of 100 weight parts, releasing agent can be used about 0.01-8 weight part.In described scope, for the tackiness of reflector, can not degenerate.Preferably, use about 1-7 weight part.
Heat-resisting or the cold tolerance of additive is outstanding, and approximately-50 ℃ to the 250 ℃ elasticity that maintain widely product in temperature range.As additive, can use the structure that comprises crosslinked line style dimethicone.
For example, additive can be used the fine silicone powder of the structural unit that comprises following formula 5 expressions.Or additive can be used the mixing silicone powder after the silicone resin coating of following formula 6 for fine silicone powder that following formula 5 is represented.
< chemical formula 5>
< chemical formula 6>
（RSiO
3/2）n
(wherein, R is methyl, phenyl, vinyl or hydrogen.N is 2 to 10000 integer)
The median size of described silicone powder (D50) can be about 0.8 to 40 μ m.
With respect to total 100 weight parts of resin combination for heat curing-type luminous reflectance, additive can comprise about 0.01-10 weight part.In described scope, forming composition can impact-absorbing, and has the effect that improves wear resistance and release property.Preferably, can comprise about 0.1-7 weight part.
Thermocurable luminous reflectance according to the present invention except epoxy resin, solidifying agent, curing catalyst, inorganic filler, white pigment, releasing agent and additive, can also comprise other various additives with resin combination.For example, from the surface tackiness improving between resin and inorganic filler and white pigment, consider, can use as required coupling agent.For coupling agent, have no particular limits, can use silane coupling agent, titanate coupling agent.As silane coupling agent, can use epoxy silane class, aminosilane class, cationic silane class, vinyl silanes class, silicon Acrylote alkanes, hydrosulphonyl silane class etc.Coupling agent should be considered the surface coverage amount to inorganic filler, thereby makes suitable adjustment.Coupling agent is preferably below approximately 5 % by weight of resin combination.Except coupling agent, also can comprise the additives such as antioxidant, ion trap agent.
According to another aspect of the invention, provide the preparation method of a kind of heat curing-type luminous reflectance with resin combination.Described method can be that described epoxy resin, solidifying agent, curing catalyst, inorganic filler and white pigment are mixed and prepared, but hybrid mode or condition etc. is had no particular limits.Can adopt general preparation method, with devices such as mixing roll, compressor, kneader, roll, extrusion machines, various compositions are mixing, the mixing thing obtaining is prepared by method cooling and that pulverize.For compounding process, have no particular limits, can carry out melting mixing, and the temperature and time can adjust melting mixing according to the kind of various use compositions or proportional quantity time.
As a concrete example, although the not restriction of built-up sequence for each composition, but for the mixture that is mixed with epoxy resin, solidifying agent, releasing agent and additive can be melted, can maintain predetermined temperature (for example about 100-150 ℃), thereby obtain aqueous molten mixture.The molten mixture obtaining is cooled to 30-60 ℃.Drop into curing catalyst and various other raw materials such as solid state powder additive, white pigment and inorganic filler that melting does not occur, carry out melting mixing process.Melting mixing process maintains mixture under the condition of about 30-50 ℃, preferably maintains under the temperature condition of about 35-45 ℃, and with about 50-300rpm, mixing about 30-180 minute.If melting mixing deficiency of time in the time of 30 minutes, can make the dispersiveness of mixture low; And while surpassing 180 minutes, the reaction heat producing during due to composition react, is difficult to control reaction, and likely produces gel in mixture.Although to the not restriction of the built-up sequence of each composition, preferably first by after epoxy resin, solidifying agent, releasing agent and various additive pre-mixing, then add curing catalyst, white pigment, inorganic filler and the solid additives of melting do not occur.
According to another aspect of the invention, provide a kind of optical semiconductor lift-launch reflector.Described optical semiconductor carries and can with resin combination, consist of heat curing-type luminous reflectance of the present invention with reflector.Particularly, optical semiconductor carries the recess that reflector has at least more than one, and at least in the inner side of described recess, comprises the reflector that the resin combination used by heat curing-type luminous reflectance of the present invention forms.
According to another aspect of the invention, provide a kind of optical semiconductor to carry the preparation method with reflector.Described method comprises: by described heat curing-type luminous reflectance, with resin combination, form the step that described optical semiconductor carries the inner side of reflector.Particularly, can prepare resin combination or its flat-plate molded body that heat curing-type luminous reflectance is used by transfer molding.For preparing optical semiconductor lift-launch reflector, can first from tinsel, by known methods such as punching press or etchings, form metal winding displacement.At this metal winding displacement (lead frame), implement nickel plating/silver.Then this metal winding displacement is disposed in mould, from the resin injection mouth of mould by the solute of heat curing-type of the present invention resin combination (being flat-plate molded body) for luminous reflectance.Afterwards, by the resin combination injecting, with the about 145-190 of die temperature ℃, the about 10-80Kgf/cm of forming pressure
2, separated from mould after about 100-240 is cured second, with the about 120-180 ℃ of solidification value, carry out the thermofixation of about 1-5 hour.
And, on the metal winding displacement (lead frame) of process removal optical semiconductor device, after operation such as Organic pollutants such as resin burrs, for reaching, improve the reflectivity of photosemiconductor and the object maintaining for a long time, to carry the predetermined position of the recess in region as optical semiconductor, implement again nickel plating/silver, the reflective mirror that wherein said recess consists of with the cured article of resin combination heat curing-type luminous reflectance around.
According to another aspect of the invention, provide and comprise that described optical semiconductor carries the optical semiconductor device with reflector.Described optical semiconductor device can comprise: described optical semiconductor lift-launch reflector; Be equipped on optical semiconductor and carry the optical semiconductor with the recess bottom surface of reflector; And for covering optical semiconductor, be formed in recess the transparent sealing resin layer that contains fluor.As described semiconductor element, can use LED.
Embodiment
Below, by the preferred embodiments of the present invention, by more detailed description formation of the present invention and effect.But it can not limit the present invention with this with any reason only as preferred exemplary of the present invention.
Not being recorded in this content, is that those skilled in the art can weigh and obtain through sufficient technology, therefore repeats no more.
Details are as follows for the concrete composition using in following embodiment and comparative example.
(1) epoxy resin has been used TEPIC-S(nissan chemical).
(2) solidifying agent has been used the new Japanese physical chemistry of MH-700G().
(3-1) curing catalyst has been used PEP550(4 unit alcohol) (BASF AG).
(3-2) curing catalyst has been used TPP-PB(to preserve the phosphor catalyst of photoinitiator chemical).
(4) inorganic filler has been used SiO
2(median size (D50) 1 μ m: the mixture of the weight part of the 1:1 of median size (D50) 22 μ m).
(5) white pigment has been used TiO
2(median size 0.17 μ m).
(6) releasing agent has been used PED-522(Clariant chemical industry).
(7) additive has been used KBM-403(epoxy silane) (SHIN-ETSU HANTOTAI's chemical industry).
(8) thermoplastic resin 1 has been used PA-9T TA-112(Kuraray company); Thermoplastic resin 2 has been used PA-9T TA-113(Kuraray company); Thermoplastic resin 3 has been used PA-9T TA-124(Kuraray company).
Embodiment 1-3
Content to record in following table 1 is added, and the mixture of epoxy resin, solidifying agent, releasing agent and additive is heated to 120 ℃ and carries out melting mixing.The temperature of the mixture obtaining is cooled to 40 ℃.The content of recording with following table 1 adds white pigment, curing catalyst and inorganic filler.Make the temperature of the mixture of acquisition maintain 35 ℃, with 100rpm, mix approximately 180 minutes.The mixture of acquisition is packed in dish, and in the baking box of 70 ℃, maturation, after approximately 3 hours, utilizes transfer molding machine under 150 ℃ of conditions, to carry out approximately 240 seconds, thereby prepares each test piece.
Comparative example 1-4
Except changing in following table 1 composition of content, all with the identical method of above-described embodiment, prepare composition, and prepare sample.
Table 1
Comparative example 5
Be applicable to the polyamide-based thermoplastic resin 1 with high heat resistance of this area of reflector for 0.5 watt of level LED luminous reflectance, in 300 ℃ of moulds, utilize the method for spray up n. to prepare test piece.
Comparative example 6-7
Comparative example 6-7 is except using respectively thermoplastic resin 2-3 to substitute the thermoplastic resin 1 of above-mentioned comparative example 5, adopting identical method to prepare test piece.
Experimental example: physical property evaluation
For the test piece of preparing in described embodiment and comparative example, evaluate following physicals, its result is as described in Table 2.
< test method for physical property >
(1) helicoidal flow length (S/F (Spiral flow length)) (inch): utilize EMMI Standard Module, for the composition of preparing in described embodiment and comparative example, detecting in die temperature is mobility during transfer molding under the condition of 150 ℃.In addition, in 70 ℃ of maturation processes, detected according to the S/F of maturation time.
(2) gelation time (G/T, gelation time) (second): by the composition of preparing in appropriate described embodiment and comparative example, be placed on the hot plate of 150 ℃ and react, detect from starting to the time that gelation occurs.In addition, in 70 ℃ of maturation processes, detected according to the G/T of maturation time.
(3) hot hardness (shore a hardness, Shore-A): for the composition of preparing in described embodiment and comparative example, utilize transfer molding machine, the die temperature of 150 ℃, make 50mm * 50mm * 3mm(long * wide * thick) test piece after 240 seconds, on the mould of 150 ℃, detect hardness.
(4) luminous reflectance factor (Reflectance, R) is (%): 50mm * 50mm * 1mm(is long * wide * thick) test piece, under 150 ℃ of conditions, transfer molding is approximately 240 seconds, and solidifies approximately 3 hours under 150 ℃ of conditions.Utilize V-670 spectrograph (JASCO company) to be determined at the initial luminous reflectance factor under 430nm.Then, under 180 ℃ of conditions, thermal treatment is approximately 168 hours, and under 430nm, measures luminous reflectance factor again.Fig. 1 shows for the composition of embodiment 1-3 and the composition of comparative example 4, thermal treatment after approximately 168 hours under 180 ℃ of conditions, the luminous reflectance factor changing with digestion time under 430nm.Fig. 2 shows the test piece of preparing for the composition of embodiment 1-3 and the composition of comparative example 5-7, thermal treatment after approximately 168 hours under 180 ℃ of conditions, the luminous reflectance factor changing with digestion time under 430nm.
(5) anti-discoloration (sustainment rate of luminous reflectance factor) (%): utilize the luminous reflectance factor of described detection and following formula, calculate anti-discoloration (sustainment rate of luminous reflectance factor).
Luminous reflectance factor * 100 before the luminous reflectance factor/thermal treatment of the sustainment rate of luminous reflectance factor (%)=180 ℃ of thermal treatments after approximately 168 hours
(6) peel off evaluation: long * wide * thick at 3mm * 2.5mm * 2mm() the contact site dipping water-base ink of cup-shaped products formed after, confirm to have the infiltration of the ink not caused by capillary phenomenon.During ink bleed, with zero, represent, not infiltration time with Χ, represent.
Table 2
As shown in table 2, do not add the comparative example 1 of curing catalyst of the present invention, more difficult reacting in the maturation temperature of 70 ℃, even also existed with its uncured state after 3 hours, is therefore difficult to preparation semi-cured state (B-Stage).Epoxy resin with respect to 100 weight parts, the addition of curing catalyst is the composition of the comparative example 2 of 2 weight parts, different from the comparative example 1 that does not comprise curing catalyst, although there is reaction at the temperature of 70 ℃, S/F is that 103 inches of above, G/T are 100 seconds, although be prepared into semi-cured state, but after transfer molding, because hot hardness is 10, there is the phenomenon bonding with mould, be difficult to be prepared as the test piece of evaluating physical property, cause detecting luminous reflectance factor and peel off evaluation.When the epoxy resin of 100 weight parts comprises the curing catalyst of 50 weight parts, although there is reaction in identical maturation temperature, but there is not the sufficient crosslinking reaction of composition, therefore the hot hardness after transfer molding is for being low to moderate 12, be difficult to equally be prepared into semi-cured state, cause detecting luminous reflectance factor and peel off evaluation.On the contrary, in embodiment 1,2 and 3, at 70 ℃ of maturation temperature, react, can be prepared into semi-cured state, the hot hardness after transfer molding reaches more than 50, for preparing test piece without any problem.Initial luminous reflectance factor is all higher in embodiment 1,2 and 3, and reached more than 90%, and be determined at the luminous reflectance factor of 180 ℃ of thermal treatments after approximately 168 hours, the result demonstration of judgement anti-discoloration, embodiment 1,2 and 3 is all shown as more than 70%.In the comparative example 4 of the phosphorus curing catalyst that use comprises aromatic group, at the maturation temperature of 70 ℃, there is sufficient reaction, and be prepared into semi-cured state after 30 minutes.During transfer molding, because its hot hardness is higher, test piece is prepared without any difficulty, and does not also occur peeling.But for anti-discoloration, although the initial luminous reflectance factor detecting is higher, the luminous reflectance factor after high-temperature heat treatment is significantly lower than the present invention.This is due to after high-temperature heat treatment, and the variable color situations such as xanthochromia occur, and therefore cannot maintain initial luminous reflectance factor, causes anti-discoloration unsatisfactory.And, as shown in the result of comparative example 5-7 and Fig. 2, by can be used in the art luminous reflectance with reflector, there is test piece prepared by the thermoplastic resin of the polyamide-based series of high heat resistance, after Overheating Treatment, its luminous reflectance factor equally also occurs to decline rapidly, and therefore known its anti-discoloration is unsatisfactory.
In addition, for the composition of preparing, be determined at the S/F and the G/T that under 70 ℃ of conditions, with the maturation time, change, and result as shown in Table 3 and Table 4 in described embodiment and comparative example.
Table 3
Table 4
As shown above, composition of the present invention can be prepared into and have suitable S/F value and the semi-cured state of G/T value; On the contrary, the composition of comparative example 1-3 occurs uncured, or just preparing semi-cured state does not at last possess suitable S/F value and G/T value yet.Comparative example 4, after 0.5 hour, within the time faster, is prepared into semi-cured state, and it has suitable S/F value and G/T value, and afterwards, because it does not have mobility, and has carried out gelation, therefore causes detecting its G/T value.
Industrial applicibility
The invention provides a kind of excellent anti-discoloration that obtains that has, therefore the heat curing-type luminous reflectance resin combination of flavescence or variable color can not occur.In addition, the invention provides a kind of long-time exposure and at high temperature, also can not make the reflective heat curing-type luminous reflectance resin combination that rate reduces of penetrating.
Be more than that embodiments of the invention and accompanying drawing are described, but the present invention is not limited to described embodiment and accompanying drawing, can be prepared into multiple different form.The technician with conventional knowledge in the technical field of the invention, in the situation that do not change the essential feature of technological thought of the present invention, can implement multiple other concrete form.Therefore, as described in embodiment be interpreted as inventing whole illustration, rather than the restriction to this.
Claims (20)
1. a heat curing-type luminous reflectance resin combination, its comprise there are approximately 2 above hydroxyls polyvalent alcohol as curing catalyst, the test piece of being prepared by described composition is about more than 70% for the sustainment rate of the luminous reflectance factor representing with following formula 1;
< formula 1>
Luminous reflectance factor * 100 before the luminous reflectance factor/thermal treatment of the sustainment rate of luminous reflectance factor (%)=180 ℃ of thermal treatments after approximately 168 hours.
2. heat curing-type luminous reflectance resin combination according to claim 1, is characterized in that, described hydroxyl is about more than 3.
3. heat curing-type luminous reflectance resin combination according to claim 1, is characterized in that, described composition, after transfer molding, solidifies approximately 3 hours at 150 ℃, then the sustainment rate of the luminous reflectance factor after approximately 168 hours is about more than 70% 180 ℃ of thermal treatments.
4. heat curing-type luminous reflectance resin combination according to claim 1, is characterized in that, described composition when transfer molding, helicoidal flow length (Spiral Flow Length(S/F)) be about 15-45 inch.
5. heat curing-type luminous reflectance resin combination according to claim 1, is characterized in that, described composition when transfer molding, gelation time (gelation time(G/T)) be about 30-70 second.
6. heat curing-type luminous reflectance resin combination according to claim 1, is characterized in that, the hydroxyl equivalent of described curing catalyst is about more than 30.
7. heat curing-type luminous reflectance resin combination according to claim 1, is characterized in that, described curing catalyst does not comprise aromatic group.
8. heat curing-type luminous reflectance resin combination according to claim 1, is characterized in that, described curing catalyst has the structure of following chemical formula 3:
< chemical formula 3>
OH-(CH
2)
m-[CR
1-OH]
n-(CH
2)
p-OH
(in above-mentioned formula, R
1hydrogen or the line style of carbonatoms 1-30 or the alkyl of ramiform; N is the integer of 0-20; M and p are the integers of 0-10 independently.But n, m and p are except 0 situation entirely).
9. heat curing-type luminous reflectance resin combination according to claim 1, is characterized in that, described composition comprises described fixed line promotor, epoxy resin, solidifying agent, inorganic filler and white pigment.
10. heat curing-type luminous reflectance resin combination according to claim 9, is characterized in that, with respect to the described epoxy resin of 100 weight parts, curing catalyst comprises about 3-49 weight part.
11. heat curing-type luminous reflectance resin combinations according to claim 9, is characterized in that, described epoxy resin does not comprise aromatic group.
12. heat curing-type luminous reflectance resin combinations according to claim 9, is characterized in that, described solidifying agent does not comprise aromatic group.
13. heat curing-type luminous reflectance resin combinations according to claim 9, is characterized in that, in described composition, the ratio of white pigment and inorganic filler is about 1:0.1 to 1:4 weight ratio.
14. heat curing-type luminous reflectance resin combinations according to claim 9, it is characterized in that the inorganic filler that described inorganic filler comprises the not enough approximately 10 μ m of median size (D50) and the mixture that median size (D50) is about the inorganic filler of 10-35 μ m.
15. heat curing-type luminous reflectance resin combinations according to claim 9, is characterized in that, described composition also can comprise more than one that select in the group being comprised of releasing agent and additive.
16. heat curing-type luminous reflectance resin combinations according to claim 15, is characterized in that, described additive has the structure of crosslinked line style dimethicone.
17. 1 kinds of heat curing-type luminous reflectance preparation method of resin combination, it comprises: by epoxy resin and solidifying agent melting mixing; And in described mixture, curing catalyst, inorganic filler and the white pigment that interpolation comprises the polyvalent alcohol with 2 above hydroxyls is with the step of melting mixing.
The preparation method of resin combination for 18. heat curing-type luminous reflectance according to claim 17, is characterized in that, described melting mixing step is at the temperature of about 30-50 ℃, carries out approximately 30 to 180 minutes.
19. 1 kinds of optical semiconductor lift-launch reflectors, it comprises the thermohardening type luminous reflectance resin combination according to any one in claim 1-16.
20. 1 kinds of optical semiconductor devices, it comprises the optical semiconductor lift-launch reflector described in claim 19.
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| KR1020110047065A KR101092015B1 (en) | 2011-05-03 | 2011-05-18 | Thermosetting resin composition for light reflection, process for producing the same, substrate made therefrom for photosemiconductor element mounting, and photosemiconductor device |
| KR10-2011-0047065 | 2011-05-18 | ||
| PCT/KR2012/003792 WO2012157938A2 (en) | 2011-05-18 | 2012-05-15 | Thermosetting resin composition for light reflection, preparation method thereof, reflecting plate for loading photonic semiconductor prepared therefrom, and photonic semiconductor device containing same |
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