CN105862017A - Reagent for preventing silver of LED silver bracket from discoloring and preparation and film forming methods - Google Patents
Reagent for preventing silver of LED silver bracket from discoloring and preparation and film forming methods Download PDFInfo
- Publication number
- CN105862017A CN105862017A CN201610246337.XA CN201610246337A CN105862017A CN 105862017 A CN105862017 A CN 105862017A CN 201610246337 A CN201610246337 A CN 201610246337A CN 105862017 A CN105862017 A CN 105862017A
- Authority
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- China
- Prior art keywords
- silver
- led
- tarnish agent
- support
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 98
- 239000004332 silver Substances 0.000 title claims abstract description 98
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003153 chemical reaction reagent Substances 0.000 title abstract 5
- 239000003795 chemical substances by application Substances 0.000 claims description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 238000005538 encapsulation Methods 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 238000010276 construction Methods 0.000 claims description 6
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 241000218202 Coptis Species 0.000 claims description 3
- 235000002991 Coptis groenlandica Nutrition 0.000 claims description 3
- 239000003377 acid catalyst Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 238000001548 drop coating Methods 0.000 claims description 2
- 238000004528 spin coating Methods 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 150000001298 alcohols Chemical class 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 18
- 229910052717 sulfur Inorganic materials 0.000 abstract description 17
- 239000011593 sulfur Substances 0.000 abstract description 17
- 229920001296 polysiloxane Polymers 0.000 abstract description 13
- -1 polysiloxane Polymers 0.000 abstract description 12
- 229920005989 resin Polymers 0.000 abstract description 9
- 239000011347 resin Substances 0.000 abstract description 9
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 abstract description 9
- 229920002554 vinyl polymer Polymers 0.000 abstract description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000010409 thin film Substances 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000006087 Silane Coupling Agent Substances 0.000 abstract 3
- 239000002131 composite material Substances 0.000 abstract 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract 1
- 229910052737 gold Inorganic materials 0.000 abstract 1
- 239000010931 gold Substances 0.000 abstract 1
- 238000012858 packaging process Methods 0.000 abstract 1
- 230000002265 prevention Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 26
- 238000004806 packaging method and process Methods 0.000 description 15
- 229920003023 plastic Polymers 0.000 description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 11
- 229910000077 silane Inorganic materials 0.000 description 11
- 238000001764 infiltration Methods 0.000 description 10
- 230000008595 infiltration Effects 0.000 description 10
- 238000005987 sulfurization reaction Methods 0.000 description 9
- 238000003860 storage Methods 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000003292 glue Substances 0.000 description 5
- 208000003351 Melanosis Diseases 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 238000010025 steaming Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000001802 infusion Methods 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 3
- 210000004127 vitreous body Anatomy 0.000 description 3
- WGRZHLPEQDVPET-UHFFFAOYSA-N 2-methoxyethoxysilane Chemical compound COCCO[SiH3] WGRZHLPEQDVPET-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 229920001709 polysilazane Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012956 testing procedure Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910052946 acanthite Inorganic materials 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000003487 anti-permeability effect Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920006268 silicone film Polymers 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- FSJWWSXPIWGYKC-UHFFFAOYSA-M silver;silver;sulfanide Chemical compound [SH-].[Ag].[Ag+] FSJWWSXPIWGYKC-UHFFFAOYSA-M 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/02—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using non-aqueous solutions
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/58—Treatment of other metallic material
-
- 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
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials For Medical Uses (AREA)
- Media Introduction/Drainage Providing Device (AREA)
- Led Device Packages (AREA)
Abstract
The invention discloses a reagent for preventing silver of an LED silver bracket from discoloring and preparation and film forming methods. The reagent for preventing silver from discoloring is prepared from a sulfydryl-containing silane coupling agent and one or two vinyl-containing silane coupling agents capable of being compatible with package resin. The LED silver bracket which is equipped with gold wires but is not packaged with resin is soaked into a silane coupling agent mixing solution with sulfydryl and vinyl in the end group, so that a two-layer-like polysiloxane composite thin film can be quickly generated on the silver-based surface. High bonding force can be generated between the polysiloxane composite thin film and silver, and the polysiloxane composite thin film is high in compatibility with the package resin on the surface. The reagent for preventing silver from discoloring is high in sulfur prevention capacity and low in cost, and cannot affect the later packaging process; the synthesis process is simple, and the subsequent use and operation are simple and convenient; therefore, the reagent is suitable for large-scale popularization, and has the advantages of not polluting the environment and the like.
Description
Technical field
The present invention relates to a kind of method preventing silver or silver coating material sulphide discoloration easily and efficiently, particularly to LED silver
The method of support anti-sulfur variable color.
Background technology
In recent years, light emitting diode (LED) lamp is many owing to having wide, the environmental protection of energy-efficient, life-span length, range etc.
Advantage, whole LED industry all obtains development at full speed at home or abroad.But it is as the prolongation of use time, LED
Light can be the most dimmed, and light decay raises rapidly, and luminous flux is decreased obviously, and the service life of lamp shortens, and serious even generation is dead
Lamp phenomenon.This problem seriously becomes to increasingly sharpen along with air pollution.Trace it to its cause, be owing to LED the most generally makes
With silver or silver coating material as stent base, for reflective and heat conduction.And ag material easily variable color in atmosphere, the most right
Sulfur in air is especially sensitive, easily generates dark-coloured Ag2S, causes silver layer blackening, thus causes this phenomenon above-mentioned.
For LED this problem of SERS substrate variable color, the most conventional solution has two kinds, and one is to be covered by modification
Potting resin on silver support, reports by optimizing improving its overall crosslink density, such as patent CN 102965069 A
The ratio of organic silicon packaging glue phenyl, vinyl and vinyl MQ resin, improves the anti-cure efficiency of packaging plastic.Another kind of
Scheme is by directly covering one layer of fine and close protecting film in LED element, then encapsulates the mode of silicone resin to improve silver
Anti-sulfur ability.Such as patent CN 104576901 A by putting on the coating of polysilazane material at LED silver substrate surface
To improve the anti-sulfur ability of LED element.Front kind of method is easy and simple to handle, but owing to the raising of organic silica gel density can cause LED
The decline of luminous flux, and its barrier properties for gases of molecular encapsulation is the strongest, it is impossible to stop the discoloration problem of SERS substrate completely.Rear kind side
Method can improve the anti-sulfur performance of LED element well, but its polysilazane synthesis technique is complicated, operating process is loaded down with trivial details, carries
High production cost.So the most urgently the exploitation the most anti-sulfur of one is functional, environmentally friendly, synthesis can be made again simultaneously
Process and use process operation are simple, with low cost, and don't affect the anti-silver tarnish agent of encapsulation process follow-up for LED.
Summary of the invention
It is an object of the invention to provide preparation and the film build method of a kind of LED silver support anti-silver tarnish agent, significantly carry
High LED money base anti-sulfur performance.
The present invention is achieved by the following technical solutions.
A kind of LED silver support anti-silver tarnish agent of the present invention, uses two or more energy compatible simultaneously
Silane coupler as main component；One of which silane coupler is the silane coupler of band sulfydryl, utilizes such coupling
The sulfydryl of agent end and SERS substrate bonding, make to combine between silane coupler and money base is more tight, and arrangement is more orderly, increases
Add the adhesive force between itself and silver；By being re-introduced into the silane coupled of one or both band vinyls that can be compatible with packaging plastic
Agent, on the one hand can improve the light transmittance of packaging plastic；Another aspect can effectively stop brings packaging plastic because introducing sulfydryl
The change of character.
The film build method of a kind of LED silver support anti-silver tarnish agent, will accomplish fluently gold thread but the LED silver support of non-resin-encapsulated
Immerse in the end group silane coupler mixed solution containing sulfydryl and vinyl, utilize the characteristic being bonded between money base with sulfydryl, make
The silane coupler obtaining band sulfydryl is enriched with at silver layer surface, and the silane coupler of band vinyl tends to upper strata enrichment and (has energy
The characteristic compatible with organic packages resin), recycling silane coupler can the characteristic of at high temperature dehydration polymerization simultaneously so that on
State silane coupler and can be quickly generated a kind of polysiloxanes laminated film approximating bilayer on money base surface.This polysiloxanes is combined
Thin film not only and is formed between silver has good adhesive force, and can have good compatibility with surface encapsulation resin compatibility again
Property.Finally on the polysiloxanes laminated film that LED money base surface is formed, carry out organic resin encapsulation again.
A kind of LED silver support anti-silver tarnish agent of the present invention, including following (1), (2) two kinds of construction units:
(1) (2)
Wherein, R is-CH2Or-C2H4；R1=R2=R3Time, R1、R2And R3May be selected to be-OC2H5Or-OCH3；R1=R2Time, R1And R2Can
It is chosen as-OC2H5Or-OCH3, R3May be selected to be-CH3。
R4=R5=R6Time, R4、R5And R6May be selected to be-Cl ,-OC2H5、-OCH3、-OC2H4OCH3Or-OCOCH3；R4=R5=-Cl
Time, R6=-CH3。
A kind of LED silver support anti-silver tarnish agent of the present invention, by the ratio of two kinds of solution 15-25:1 by volume of A, B
Example is formulated.
Described solution A includes said structure unit (1), catalysts and solvents.
Preferably, the mass percent of each material of described solution A is:
Above-mentioned construction unit (1): 0.1-5.0%；
Catalyst: 1.0-5.0%；
Solvent: 90.0-98.9%.
Described B solution includes said structure unit (2), catalysts and solvents.
Preferably, the mass percent of each material of described B solution is:
Above-mentioned construction unit (2): 10.0-20.0%；
Catalyst: 1.0-5.0%；
Solvent: 75.0-89.0%.
Described catalyst is acid catalyst, preferably the one or two kinds of in formic acid, acetic acid, dilute hydrochloric acid or dilute sulfuric acid with
On.
Described solvent can be water, the one or two kinds of in the alcohol organic solvent such as methanol, ethanol, isopropanol, n-butyl alcohol
Above.
LED silver support of the present invention anti-silver tarnish agent can use the various ways film forming such as drop coating, spin coating, immersion, preferably
Ground, uses the mode soaked, and adopting in this way can be convenient, simple with large-scale use.
The method of LED silver support of the present invention anti-silver tarnish agent film forming, it concretely comprises the following steps: will accomplish fluently gold thread but
The LED silver support of non-resin-encapsulated immerses in above-mentioned anti-silver tarnish agent, takes out after immersion, is placed in 100-150 DEG C of baking oven and is dried
10-60 minute, take out.
Compared with prior art, it is an advantage of the current invention that:
The anti-silver tarnish agent the most anti-sulfur ability of the present invention is good, with low cost, do not affect later stage encapsulation process, building-up process letter
Single, follow-up use is easy and simple to handle, be suitable for large-scale promotion, but also environment will not be produced the advantages such as pollution.
The polysiloxanes laminated film formed by the anti-silver tarnish agent of the present invention not only has good anti-sulfur performance, height
Permeability, and introduce sulfydryl by end and be coordinated with money base surface silver, to such an extent as to have between the silicone film and the silver that are formed
Good adhesive force.
Good by showing as between polysiloxanes laminated film and upper strata packaging plastic that the anti-silver tarnish agent of the present invention is formed
Good compatibility.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that the present invention forms polysiloxanes laminated film on LED money base surface, the most square dotted line frame generation
Table packaging plastic.
Fig. 2 is the present invention concrete apparent figure of anti-sulfur effect, and the most from top to bottom, from left to right five width figures are respectively sulfuration 0
Minute, 15 minutes, 24 hours, 36 hours, the outside drawing of 48 hours.First the representing for embodiment 10 of melanism in the most every width figure
LED money base support, remaining represents embodiment 7-embodiment 9 respectively.
Fig. 3 is the concrete outward appearance presentation figure of infiltration after red ink steaming and decocting of the present invention, and wherein two, the left side is embodiment 10
Infiltration situation, three, the right is followed successively by the infiltration situation of embodiment 7-9 from top to bottom, and wherein between packaging plastic and money base, dead color is got over
Deeply represent infiltration situation the most serious.
Detailed description of the invention
The present invention utilize two or more with the silane coupler of different functional groups, self be hydrolyzed into silanol and by
After certain proportion preparation, high temperature dehydration is polymerized, and forms one layer of fine and close polysiloxanes laminated film.Formed by the present invention this
Kind of fine and close polysiloxanes laminated film can not only and money base between form good adhesive force, and do not affecting later stage encapsulation
In the case of glue encapsulation, remain excellent anti-sulfur performance.
According to the present invention, the polysiloxanes laminated film formed on LED money base as previously mentioned is made by the steps:
The preparation 2. using method 3. film formation step of the most anti-silver tarnish solution.
Below by combining instantiation, the present invention is further illustrated, but not thereby limiting the invention.
Material therefor of the present invention, in the case of without specified otherwise, all can be either commercially available by public.Meanwhile, with
LED silver support used in lower embodiment, is the most commercially available, before use, the most further its money base surface is done anti-sulfur
Processing, general tree size is any limitation as and requirement.In embodiment, packaging plastic used is general commercial BQ-4138A/B model
Glue.
One, LED silver support anti-silver tarnish agent component preparation.
Embodiment 1.
LED silver support anti-silver tarnish agent component A is prepared: take 40mL ethanol in 100mL beaker, drips 3.5mL deionization
Water, 1.6mL acetic acid, shake up, add 0.7mL3-mercaptopropyltriethoxysilane, stirring (room temperature, middling speed) 18 hours.Permissible
Dropping on microscope slide by taking a solution, 100 DEG C of drying in oven, if transparent vitreous body, explanation can use.Prepare
After, room storage 15 DEG C is stand-by.Described solution is A1.
LED silver support anti-silver tarnish agent B component is prepared: take 4mL ethanol in 20mL bottle, inside dropping 3mL deionization
Water, 1.2mL vinyl three (2-methoxy ethoxy) silane, stand 24h.After preparing, room storage 15 DEG C) stand-by.Described molten
Liquid is B1.
Embodiment 2.
LED silver support anti-silver tarnish agent component A is prepared: take 40mL ethanol in 100mL beaker, drips 5mL deionized water,
2.5mL acetic acid, shakes up, and adds 1.0mL3-mercaptopropyltriethoxysilane, stirring (room temperature, middling speed) 20 hours.Can pass through
Taking a solution and drop on microscope slide, 150 DEG C of drying in oven, if transparent vitreous body, explanation can use.After preparing, room
Temperature storage 25 DEG C is stand-by.Described solution is A2.
LED silver support anti-silver tarnish agent B component is prepared: take 4mL ethanol in 20mL bottle, drips 3mL deionized water,
1.2mL vinyl three (2-methoxy ethoxy) silane, stands 24h.After preparing, room storage 25 DEG C is stand-by.Described solution is
B2。
Embodiment 3.
LED silver support anti-silver tarnish agent component A is prepared: take 40mL methanol in 100mL beaker, drips 5mL deionized water,
1.6mL formic acid, shakes up, and adds 1.0mL3-mercaptopropyl trimethoxysilane, stirring (room temperature, middling speed) 24 hours.Can pass through
Taking a solution and drop on microscope slide, 100 DEG C of drying in oven, if there being transparent vitreous body, explanation can use.After preparing, room
20 DEG C of storages of temperature are stand-by.Described solution is A3.
LED silver support anti-silver tarnish agent B component is prepared: take 4mL ethanol in bottle, inside dropping 3mL deionized water,
0.6mL acetic acid, 1.2mL VTES, stand 24h.After preparing, room temperature 20 DEG C storage is stand-by.Described solution is
B3。
Two, the preparation of LED silver support anti-silver tarnish agent.
Embodiment 4.
Take above-mentioned A1 solution 4mL, add 0.35mLB1 solution inside, stir 0.5 hour.After preparing, room temperature 15 DEG C)
Store stand-by.Described is C1 for anti-silver tarnish agent.
Embodiment 5.
Take above-mentioned A2 solution 4mL, add 0.50mLB2 solution inside, stir 2 hours.After preparing, room temperature 25 DEG C storage
Hide stand-by.Described is C2 for anti-silver tarnish agent.
Embodiment 6.
Take above-mentioned A3 solution 4mL, add 0.2mLB2 solution inside, stir 1 hour.After preparing, room temperature 20 DEG C storage
Stand-by.Described is C2 for anti-silver tarnish agent.
Three, film forming preparation process.
Embodiment 7.
Use the anti-silver tarnish agent C1 for preparing of embodiment 4, by infusion method, LED silver support is steeped into wherein, 5-10 minute
Rear taking-up, after be placed directly within 100-150 DEG C of oven for drying, take out after 10-60 minute, as far as possible retaining groove solution during this
Do not spill.
Embodiment 8.
Use the anti-silver tarnish agent C2 for preparing of embodiment 5, by infusion method, LED silver support is steeped into wherein, 5-10 minute
Rear taking-up, after be placed directly within 100-150 DEG C of oven for drying, take out after 10-60 minute, as far as possible retaining groove solution during this
Do not spill.
Embodiment 9.
Use the anti-silver tarnish agent C3 for preparing of embodiment 6, by infusion method, LED silver support is steeped into wherein, 5-10 minute
Rear taking-up, after be placed directly within 100-150 DEG C of oven for drying, take out after 10-60 minute, as far as possible retaining groove solution during this
Do not spill.
The anti-sulphuring treatment LED silver support that is ready for of embodiment 7-9 is divided into two parts, part polyorganosiloxane resin
Being packaged, package curing step is: 80 DEG C/1 hour+150 DEG C/3 hours.Another part does not encapsulates.
Comparative example 10.
LED silver support is without anti-vulcanizing treatment, and a part directly uses the encapsulation of silicone encapsulation glue, and package curing walks
Suddenly it is: 80 DEG C/1 hour+150 DEG C/3 hours.Another part does not encapsulates.
Embodiment 11: contrast anti-cure efficiency.
Detecting LED silver support (being not added with packaging plastic) the anti-cure efficiency in embodiment 7-10, detection method is: sulfur
China's accelerated cure experiment.
Concrete testing procedure is as follows: LED silver support (the being not added with packaging plastic) unification in embodiment 7-10 is put into 500mL close
In envelope vial, bottle built with 20g sulfur, 0.2g deionized water, under 100 DEG C of air-proof conditions, after sulfuration points 15 minutes, 24 little
Time, 36 hours, 48 hours postfixed points take out flowers of sulfur bottle, treat near room temperature respectively, take out LED silver support control cure degree, tool
Body sulfuration situation see table:
| Money base sulfuration situation/sample | Example 7 | Example 8 | Example 9 | Example 10 |
| Vulcanize 15 minutes money base surface conditions | Keep light | Keep light | Keep light | Blackening completely |
| Vulcanize 24 hours money base surface conditions | Keep light | Keep light | Keep light | |
| Vulcanize 36 hours money base surface conditions | Keep light | Keep light | Keep light | |
| Vulcanize 48 hours money base surface conditions | Corner melanism part | Corner melanism part | Corner melanism part |
Concrete appearance after sulfuration, it is seen that accompanying drawing 2.
Embodiment 12: after control cure, light decay situation measures.
Detecting LED silver support (adding packaging plastic) the anti-cure efficiency in embodiment 7-10, detection method is: through sulfur
After China's accelerated cure experiment, then carry out light decay determination experiment.
Concrete testing procedure is as follows: put into 500mL sealing by unified for LED silver support (adding packaging plastic) in embodiment 7-10
In vial, bottle built with 20g sulfur, 0.2g deionized water, under 100 DEG C of air-proof conditions, take out flowers of sulfur bottle every 2h, treat by
To room temperature, take out LED silver support light-metering and decline.Concrete light decay data step by step see table:
| Light decay/sample | Example 7 | Example 8 | Example 9 | Example 10 |
| Light decay after 2h sulfuration | 4.6% | 4.4% | 4.8% | 53.0%(lamp in heaven) |
| Light decay step by step after 4h sulfuration | 1.7% | 1.9% | 1.7% | |
| Light decay step by step after 6h sulfuration | 1.5% | 1.3% | 1.6% | |
| Light decay after 8h sulfuration step by step | 1.1% | 1.5% | 1.5% |
Embodiment 13: high temperature red ink is tested, the anti-permeability after contrast packaging plastic solidification.
By unified for LED silver support (adding packaging plastic) in the embodiment 7-10 rustless steel putting into the 500mL equipped with red ink
In Bei, high temperature steaming, test is by the permeability that whether can affect surface encapsulation glue after money base face seal layer protecting film.
Concrete test condition is as follows: 170 DEG C of red ink solution (red ink: ethanol=1:1) steaming and decocting 1 hour.The most impermeable
Situation see table:
| Permeability/sample | Example 7 | Example 8 | Example 9 | Example 10 |
| Red ink infiltration situation | Medium infiltration | Medium infiltration | Medium infiltration | Heavy infiltration |
The outward appearance presentation of the concrete infiltration after red ink steaming and decocting, it is seen that accompanying drawing 3.
Claims (7)
1. a LED silver support anti-silver tarnish agent, is characterized in that including following two kinds of construction units:
(1) (2)
In formula (1), R is-CH2Or-C2H4；R1=R2=R3Time, R1、R2And R3For-OC2H5Or-OCH3；R1=R2Time, R1And R2For-
OC2H5Or-OCH3, R3For-CH3；
In formula (2), R4=R5=R6Time, R4、R5And R6For-Cl ,-OC2H5、-OCH3、-OC2H4OCH3Or-OCOCH3；R4=R5=-Cl
Time, R6=-CH3。
2. the preparation method of the LED silver support anti-silver tarnish agent described in claim 1, is characterized in that by two kinds of solution of A, B by body
The long-pending proportions than 15-25:1 forms；
Described solution A includes said structure unit (1), catalysts and solvents, and the mass percent of its each material is:
Above-mentioned construction unit (1): 0.1-5.0%；
Acid catalyst: 1.0-5.0%；
Solvent: 90.0-98.9%；
Described B solution includes said structure unit (2), catalysts and solvents, and the mass percent of its each material is:
Above-mentioned construction unit (2): 10.0-20.0%；
Acid catalyst: 1.0-5.0%；
Solvent: 75.0-89.0%.
The preparation method of LED silver support the most according to claim 2 anti-silver tarnish agent, is characterized in that described catalyst is first
More than the one or two kinds of in acid, acetic acid, dilute hydrochloric acid or dilute sulfuric acid.
The preparation method of LED silver support the most according to claim 2 anti-silver tarnish agent, it is characterized in that described solvent be water or
Alcohol organic solvent.
The preparation method of LED silver support the most according to claim 4 anti-silver tarnish agent, is characterized in that described alcohols is organic
Solvent is more than the one or two kinds of in methanol, ethanol, isopropanol, n-butyl alcohol.
6. the film build method of the LED silver support anti-silver tarnish agent described in claim 1, is characterized in that described LED silver support is prevented
Silver tarnish agent drop coating, spin coating or immersion way film forming.
Film build method the most according to claim 6, is characterized in that described immersion way is not set accomplishing fluently gold thread
The LED silver support of fat encapsulation immerses in anti-silver tarnish agent, takes out after immersion, is placed in 100-150 DEG C of baking oven dry 10-60 and divides
Clock.
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