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CN108997969A - A kind of UV-LED packaging plastic and preparation method thereof - Google Patents

A kind of UV-LED packaging plastic and preparation method thereof Download PDF

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Publication number
CN108997969A
CN108997969A CN201811074328.2A CN201811074328A CN108997969A CN 108997969 A CN108997969 A CN 108997969A CN 201811074328 A CN201811074328 A CN 201811074328A CN 108997969 A CN108997969 A CN 108997969A
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China
Prior art keywords
component
packaging plastic
methyl
adamantyl
parts
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Granted
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CN201811074328.2A
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Chinese (zh)
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CN108997969B (en
Inventor
韩小兵
谢继鹏
郑长利
黄仁杰
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Guangzhou Hui Li Electron Material Co Ltd
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Guangzhou Hui Li Electron Material Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/221Oxides; Hydroxides of metals of rare earth metal
    • C08K2003/2213Oxides; Hydroxides of metals of rare earth metal of cerium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a kind of UV-LED packaging plastics, are mixed in mass ratio for 1:1 by component A and B component;Component A includes following mass fraction ingredient: 90~98 parts of the methyl vinyl silicone containing adamantyl;0.01~0.5 part of platinum catalyst;B component includes following mass fraction ingredient: 30~50 parts of the methyl vinyl silicone containing adamantyl;50~70 parts of Methyl Hydrogen Polysiloxane Fluid containing adamantyl.It selects the methyl vinyl silicone containing adamantane of specific Average molecular formula and contains the Methyl Hydrogen Polysiloxane Fluid of adamantyl as base rubber, reaction obtains packaging plastic under the catalytic action of platinum catalyst, in terms of existing technologies, packaging plastic of the present invention refractive index with higher, good sulfuration resistant performance, excellent UV resistance.

Description

A kind of UV-LED packaging plastic and preparation method thereof
Technical field
The invention belongs to LED encapsulation fields, and in particular to a kind of UV-LED packaging plastic and preparation method thereof.
Background technique
UV-LED is one kind of LED, emits the black light of Single wavelength, generally in 400nm or less.UV-LED and traditional The features such as mercury lamp is compared, and has power and energy saving, heat loss less, and the service life is long, wavelength is relatively concentrated is a kind of novel environment-friendly type light Source, by the favor in market.Currently, the packaged type of white light LEDs is mainly continued to use in the encapsulation of UV-LED, organosilicon tree is still used For rouge as encapsulating material, but since the wavelength of UV-LED is shorter, radiation energy is higher, therefore has to the performance of encapsulating material higher Requirement.
Traditional organosilicon encapsulating material mainly has methyl silica gel and phenyl silica gel, methyl silica gel have it is heat-resisting well and UV resistance, but refractive index is relatively low, and the light extraction efficiency of LED is low, and since hardness is lower, sulfuration resistant performance is poor;Phenyl Silica gel refractive index is high, hardness is high, has preferable light extraction efficiency and sulfuration resistant performance, but its heatproof, UV resistance are poor, holds It is also easy to produce xanthochromia, it is larger to light light decay for a long time.
In conclusion needing the UV-LED packaging plastic that a kind of refractive index is high, heat resistance is good.
Summary of the invention
For overcome the deficiencies in the prior art, the present invention provides the UV-LED encapsulation that a kind of refractive index is high, heat resistance is good Glue.
Refractive index height is opposite height in this discovery, and is not specific to some specific value, and heat resistance is also relatively existing well For having a technology.
To solve the above problems, the technical solution adopted in the present invention is as follows:
A kind of UV-LED packaging plastic, is mixed in mass ratio for 1:1 by component A and B component;
Component A includes following mass fraction ingredient:
90~98 parts of methyl vinyl silicone containing adamantyl;
0.01~0.5 part of platinum catalyst;
B component includes following mass fraction ingredient:
30~50 parts of methyl vinyl silicone containing adamantyl;
50~70 parts of Methyl Hydrogen Polysiloxane Fluid containing adamantyl;
The average formula of the methyl vinyl silicone containing adamantane in component A and B component are as follows:
In the average formula of methyl vinyl silicone containing adamantane, R1, R2, R3 be methyl or adamantyl, R1, At least a kind of in R2 and R3 is adamantyl, 5≤x≤30,5≤y≤10;
The Average molecular formula of Methyl Hydrogen Polysiloxane Fluid containing adamantyl are as follows:
In the Average molecular formula of Methyl Hydrogen Polysiloxane Fluid containing adamantyl, R is one of methyl, hydrogen and adamantyl, 5 ≤z≤20。
Preferably, further include inhibitor in B component, B component includes following parts by weight ingredient:
30~50 parts of methyl vinyl silicone containing adamantyl;
50~70 parts of Methyl Hydrogen Polysiloxane Fluid containing adamantyl;
0.01~0.5 part of inhibitor.
The catalytic effect of platinum catalyst is inhibited by the way that inhibitor is added, to control reaction rate, avoids reacting It is too fast.
Preferably, inhibitor is at least one of methyl butynol, ethynylcyclohexanol and phenylbutynol.
Using methyl butynol, ethynylcyclohexanol and phenylbutynol as inhibitor, on the one hand, can effectively inhibit platinum The catalytic effect of catalyst keeps reaction rate controllable, reserves enough operating times;On the other hand, methyl butynol, acetenyl Cyclohexanol and phenylbutynol boiling point are lower, convenient for removing, prevent the performance of the remaining influence packaging plastic of inhibitor.
Preferably, platinum catalyst is platinum-vinyl silanes complex catalyst.
Preferably, platinum content is 5000ppm in platinum-vinyl silanes complex catalyst
Preferably, further include heat-resistant agent in component A, component A includes following parts by weight ingredient:
90~98 parts of methyl vinyl silicone containing adamantyl;
1~5 part of heat-resistant agent;
0.01~0.5 part of catalyst.
Enhance the heat resistance of packaging plastic by addition heat-resistant agent.
Preferably, heat-resistant agent is polysiloxane-modified nano-cerium oxide.
Polysiloxane-modified nano-cerium oxide and the preferable compatibility of methyl vinyl silicone containing adamantyl, gathers While silicone-modified nano-cerium oxide improves packaging plastic heat resistance, the performance of packaging plastic is influenced smaller.
Preferably, further include tackifier in component A, component A includes following parts by weight ingredient:
90~98 parts of methyl vinyl silicone containing adamantyl;
1~5 part of tackifier;
0.01~0.5 part of catalyst.
By adding tackifier, the bonding force of packaging plastic is improved.
Preferably, tackifier are at least one of silane coupling agent KH-560 and silane coupling agent KH-561.
Silane coupling agent KH-560 and silane coupling agent KH-561 appearance colorless are transparent, are applied in UV-LED packaging plastic, It is smaller on the influence of the light-out effect of UV-LED after solidification, the cohesive force of packaging plastic Yu bracket silver coating can be effectively improved.
The present invention also provides a kind of preparation methods of UV-LED packaging plastic, comprising the following steps:
Each ingredient in the component A of corresponding mass number is weighed, is added sequentially in de-airing mixer, is uniformly mixed up to A Component;
Each ingredient in the B component of corresponding mass number is weighed, is added sequentially in de-airing mixer, is uniformly mixed up to B Component;
By component A and B component, 1:1 in mass ratio is added in de-airing mixer, is uniformly mixed, is obtained packaging plastic.
By by reactant in component A and B component respectively premixing uniformly, then by component A and B component hybrid reaction, It avoids directly mixing all raw materials, prevents local reaction is too fast during being dispersed with stirring from reaction being caused to fail.
In terms of existing technologies, the invention has the following advantages:
The methyl vinyl silicone containing adamantane for selecting specific Average molecular formula and the methyl containing adamantyl Containing hydrogen silicone oil is as base rubber, and reaction obtains packaging plastic under the catalytic action of platinum catalyst, compared with the existing technology in for, this Invention packaging plastic refractive index with higher, good sulfuration resistant performance, excellent UV resistance.
Specific embodiment
Invention is further described in detail With reference to embodiment.
Embodiment 1
A kind of UV-LED packaging plastic, is mixed in mass ratio for 1:1 by component A and B component;
Component A includes following component:
Component A includes following component:
Methyl vinyl silicone 30g containing adamantyl;
Methyl Hydrogen Polysiloxane Fluid 69.99g containing adamantyl;
Methyl butynol 0.01g;
The present embodiment UV-LED packaging plastic preparation method the following steps are included:
A) methyl vinyl silicone of the 90g containing adamantyl, the polysiloxane-modified nano-cerium oxide of 5g (Dongguan Shandong are weighed Jump AHR-3), silane coupling agent KH-560 and 0.01g platinum-vinyl silanes complex catalyst of 4.99g (platinum content: 5000ppm), it is added sequentially in de-airing mixer, component A can be obtained by being uniformly mixed;
B) weigh Methyl Hydrogen Polysiloxane Fluid containing adamantyl of methyl vinyl silicone, 69.99g of the 30g containing adamantyl, The methyl butynol of 0.01g, is added sequentially in de-airing mixer, and B component can be obtained by being uniformly mixed;
C) by component A and B component, 1:1 in mass ratio is added in de-airing mixer, is uniformly mixed, is obtained packaging plastic.
Embodiment 2
A kind of UV-LED packaging plastic, is mixed in mass ratio for 1:1 by component A and B component;
Component A includes following component:
Component A includes following component:
Methyl vinyl silicone 49.5g containing adamantyl;
Methyl Hydrogen Polysiloxane Fluid 50g containing adamantyl;
Phenylbutynol 0.5g;
The present embodiment UV-LED packaging plastic preparation method the following steps are included:
A) methyl vinyl silicone of the 97.5g containing adamantyl, the polysiloxane-modified nano-cerium oxide (Dongguan 1g are weighed Shandong jumps AHR-3), silane coupling agent KH-561 and 0.5g platinum-vinyl silanes complex catalyst (platinum content: 5000ppm) of 1g, It is added sequentially in de-airing mixer, component A can be obtained by being uniformly mixed;
B) weigh Methyl Hydrogen Polysiloxane Fluid containing adamantyl of methyl vinyl silicone, 50g of the 49.5g containing adamantyl, The phenylbutynol of 0.5g, is added sequentially in de-airing mixer, and B component can be obtained by being uniformly mixed;
C) by component A and B component, 1:1 in mass ratio is added in de-airing mixer, is uniformly mixed, is obtained packaging plastic.
Embodiment 3
A kind of UV-LED packaging plastic, is mixed in mass ratio for 1:1 by component A and B component;
Component A includes following component:
Component A includes following component:
Methyl vinyl silicone 50g containing adamantyl;
Methyl Hydrogen Polysiloxane Fluid 49.5g containing adamantyl;
Ethynylcyclohexanol 0.5g;
The present embodiment UV-LED packaging plastic preparation method the following steps are included:
A) methyl vinyl silicone of the 90g containing adamantyl, the polysiloxane-modified nano-cerium oxide (Dongguan 4.5g are weighed Shandong jumps AHR-3), silane coupling agent KH-561 and 0.5g platinum-vinyl silanes complex catalyst (platinum content: 5000ppm) of 5g, It is added sequentially in de-airing mixer, component A can be obtained by being uniformly mixed;
B) weigh Methyl Hydrogen Polysiloxane Fluid containing adamantyl of methyl vinyl silicone, 49.5g of the 50g containing adamantyl, The ethynylcyclohexanol of 0.5g, is added sequentially in de-airing mixer, and B component can be obtained by being uniformly mixed;
C) by component A and B component, 1:1 in mass ratio is added in de-airing mixer, is uniformly mixed, is obtained packaging plastic.
Comparative example 1
A) KH-561 and 0.5g platinum-vinyl silanes complex catalyst of 94.5g methyl vinyl silicone, 5g is weighed (Pt content: 5000ppm), is added sequentially in de-airing mixer, and component A can be obtained by being uniformly mixed;
B) weigh 50g methyl vinyl silicone, 49.5g Methyl Hydrogen Polysiloxane Fluid, 0.5g ethynylcyclohexanol, successively plus Enter into de-airing mixer, B component can be obtained by being uniformly mixed;
C) by component A and B component, 1:1 in mass ratio is added in de-airing mixer, is uniformly mixed, is obtained packaging plastic.
Comparative example 2
A) KH-561 and 0.5g platinum-vinyl silanes complex catalyst of 94.5g phenyl vinyl polysiloxane, 5g are weighed (Pt content: 5000ppm), is added sequentially in de-airing mixer, and component A can be obtained by being uniformly mixed;
B) ethynylcyclohexanol of 50g phenyl vinyl polysiloxane, 49.5g phenyl hydrogen-containing silicon oil, 0.5g are weighed, successively plus Enter into de-airing mixer, B component can be obtained by being uniformly mixed;
C) by component A and B component, 1:1 in mass ratio is added in de-airing mixer, is uniformly mixed, is obtained packaging plastic.
Comparative example 3
A) methyl vinyl silicone, KH-561,4.5g BASF 1076 of 5g and 0.5g of the 90g containing adamantyl are weighed Platinum-vinyl silanes complex catalyst (Pt content: 5000ppm), is added sequentially in de-airing mixer, and being uniformly mixed can obtain Component A;
B) weigh Methyl Hydrogen Polysiloxane Fluid containing adamantyl of methyl vinyl silicone, 49.5g of the 50g containing adamantyl, The ethynylcyclohexanol of 0.5g, is added sequentially in de-airing mixer, and B component can be obtained by being uniformly mixed;
C) by component A and B component, 1:1 in mass ratio is added in de-airing mixer, is uniformly mixed, is obtained packaging plastic.
UV-LED packaging plastic prepared by Examples 1 to 3 and comparative example 1~3 is performed the following performance tests, test result is such as Shown in table 1.
(1) it refraction index test: is measured according to GB/T 6488-2008 " measuring method of liquid chemical product index of refraction ".
Sulfuration resistant test: packaging plastic point adhesive curing being placed in 1g/100ml sulphur powder environment, 80 DEG C of vulcanization 8h, measures sulphur Change the light decay situation of front and back LED.
(3) resistance to ultraviolet test: packaging plastic is used to encapsulate UV-LED (395nm) chip, lights aging under 60mA The light decay situation of front and back is lighted in 1000h, measurement.
(4) heat resistance is tested: after encapsulation adhesive curing, for 24 hours, front and back firmness change, hardness are toasted in detection for 200 DEG C of bakings It is measured according to HG/T 2413.2-1992 " the measurement Shao Er hardometer method of rubber roller apparent hardness ".
Table 1
Embodiment 1 Embodiment 2 Embodiment 3 Comparative example 1 Comparative example 2 Comparative example 3
25 DEG C of refractive index@ 1.54 1.54 1.54 1.41 1.54 1.54
Light decay after vulcanization < 3.0% < 3.0% < 3.0% 10.0% < 3.0% < 3.0%
Light light decay after 1000h < 10% < 10% < 10% < 10% 15% < 10%
200 DEG C/firmness change for 24 hours < 5D < 5D < 5D 8D 10D 9D
From table 1 it follows that comparative example and comparative example 1 illustrate, the present invention has higher relative to methyl silica gel Refractive index, light decay is lower after vulcanization, and firmness change is smaller after baking;Comparative example and comparison 2 explanation, the present invention relative to Phenyl silica gel has more preferable UV resistance, and firmness change is smaller after baking;Comparative example and the explanation of comparative example 3, relative to For conventional heat refractory agent, the present invention has better heat resistance, and firmness change is smaller after baking.
Each technical characteristic of above embodiments can be combined arbitrarily, for simplicity of description, not to above-described embodiment In each technical characteristic it is all possible combination be all described, as long as however, the combination of these technical characteristics be not present lance Shield all should be considered as described in this specification.
Only several embodiments of the present invention are expressed for above embodiments, and the description thereof is more specific and detailed, but can not Therefore it is construed as limiting the scope of the patent.It should be pointed out that for those of ordinary skill in the art, Under the premise of not departing from present inventive concept, various modifications and improvements can be made, and these are all within the scope of protection of the present invention. Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (10)

1. a kind of UV-LED packaging plastic, which is characterized in that mixed in mass ratio for 1:1 by component A and B component;
The component A includes following mass fraction ingredient:
90~98 parts of methyl vinyl silicone containing adamantyl;
0.01~0.5 part of platinum catalyst;
The B component includes following mass fraction ingredient:
30~50 parts of methyl vinyl silicone containing adamantyl;
50~70 parts of Methyl Hydrogen Polysiloxane Fluid containing adamantyl;
The average formula of methyl vinyl silicone described in the component A and B component containing adamantane are as follows:
In the average formula of the methyl vinyl silicone containing adamantane, R1、R2、R3For methyl or adamantyl, R1、R2 And R3In it is at least a kind of be adamantyl, 5≤x≤30,5≤y≤10;
The Average molecular formula of the Methyl Hydrogen Polysiloxane Fluid containing adamantyl are as follows:
In the Average molecular formula of the Methyl Hydrogen Polysiloxane Fluid containing adamantyl, R is one of methyl, hydrogen and adamantyl, 5 ≤z≤20。
2. UV-LED packaging plastic according to claim 1, which is characterized in that it further include inhibitor in the B component, it is described B component includes following parts by weight ingredient:
30~50 parts of methyl vinyl silicone containing adamantyl;
50~70 parts of Methyl Hydrogen Polysiloxane Fluid containing adamantyl;
0.01~0.5 part of inhibitor.
3. UV-LED packaging plastic according to claim 2, which is characterized in that the inhibitor is methyl butynol, acetylene At least one of cyclohexanol and phenylbutynol.
4. UV-LED packaging plastic according to claim 1, which is characterized in that the platinum catalyst is platinum-vinyl silanes Complex catalyst.
5. UV-LED packaging plastic according to claim 4, which is characterized in that the platinum-vinyl silanes complex catalyst Middle platinum content is 5000ppm.
6. UV-LED packaging plastic according to claim 1, which is characterized in that it further include heat-resistant agent in the component A, it is described Component A includes following parts by weight ingredient:
90~98 parts of methyl vinyl silicone containing adamantyl;
1~5 part of heat-resistant agent;
0.01~0.5 part of catalyst.
7. UV-LED packaging plastic according to claim 6, which is characterized in that the heat-resistant agent is polysiloxane-modified receives Rice cerium oxide.
8. UV-LED packaging plastic described in any one claim according to claim 1~7, which is characterized in that the component A In further include tackifier, the component A includes following parts by weight ingredient:
90~98 parts of methyl vinyl silicone containing adamantyl;
1~5 part of tackifier;
0.01~0.5 part of catalyst.
9. UV-LED packaging plastic according to claim 8, which is characterized in that the tackifier are silane coupling agent KH-560 At least one of with silane coupling agent KH-561.
10. a kind of preparation method of UV-LED packaging plastic as claimed in claim 8, which comprises the following steps:
A) it weighs each ingredient in the component A of corresponding mass number, is added sequentially in de-airing mixer, be uniformly mixed to obtain the final product The component A;
B) it weighs each ingredient in the B component of corresponding mass number, is added sequentially in de-airing mixer, be uniformly mixed to obtain the final product The B component;
C) by component A and B component, 1:1 in mass ratio is added in de-airing mixer, is uniformly mixed, is obtained packaging plastic.
CN201811074328.2A 2018-09-14 2018-09-14 UV-LED packaging adhesive and preparation method thereof Active CN108997969B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116656296A (en) * 2023-07-04 2023-08-29 烟台固邦新材料有限公司 A high-temperature-resistant encapsulant for electronic components and its manufacturing process
CN116656296B (en) * 2023-07-04 2025-04-18 烟台固邦新材料有限公司 A high temperature resistant packaging adhesive for electronic components and its manufacturing process

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