CN112877008B - Preparation method of high-hardness low-warpage double-layer small-particle solid-state fluorescent adhesive film - Google Patents
Preparation method of high-hardness low-warpage double-layer small-particle solid-state fluorescent adhesive film Download PDFInfo
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- CN112877008B CN112877008B CN202110075800.XA CN202110075800A CN112877008B CN 112877008 B CN112877008 B CN 112877008B CN 202110075800 A CN202110075800 A CN 202110075800A CN 112877008 B CN112877008 B CN 112877008B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives 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
- C09J183/04—Polysiloxanes
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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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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Abstract
The application relates to a fluorescent adhesive film in the field of semiconductors, in particular to a preparation method of a high-hardness low-warpage double-layer small-particle solid fluorescent adhesive film. The inner layer is a fluorescent adhesive film containing fluorescent powder and having a thickness of 30-70 mu m, and the outer layer is a transparent adhesive film containing 50-80wt% of inorganic filler and having a thickness of 30-80 mu m. The preparation method comprises the following steps: step one: a fluorescent adhesive film is coated on the release film in a scraping way; step two: a transparent adhesive film is coated on the release film in a scraping way; step three: the fluorescent adhesive film and the transparent adhesive film are compositely overlapped by using a vacuum lamination machine; step four: and (5) carrying out cutting after curing the obtained material at high temperature. The invention has the following advantages: the organic silicon transparent adhesive film added with the micron-sized inorganic filler has high hardness (Shore D80-Shore D90), scratch resistance, no deformation and no warpage, is favorable for being absorbed by a client, has excellent heat conduction and light attenuation resistance, and can be used for high-power (4.5W) LED devices.
Description
Technical Field
The application relates to a fluorescent adhesive film in the field of semiconductors, in particular to a preparation method of a high-hardness low-warpage double-layer small-particle solid fluorescent adhesive film.
Technical Field
LEDs (semiconductor light emitting diodes) are widely used in the fields of lighting, backlight, and the like because of their advantages such as low power consumption, long life, and small volume. The packaging process is a very important process in the LED manufacturing process, and has a very significant effect on the operation performance, cost, and the like of the LED.
The existing LED packaging technology mainly includes a device level packaging technology, a wafer level LED packaging (WLP) technology, a chip size level packaging CSP (Chip Scale Package) technology, and the like, which have advantages, but all have some defects at the same time. In view of this, researchers have also been working on improving LED packaging technology.
For example, US7294861B, US2014091346A1 and the like propose a technique of packaging an LED using a fluorescent tape or a fluorescent adhesive sheet. Fluorescent powder, fluorescent nanocrystals and the like are dispersed in the fluorescent adhesive tapes and the fluorescent adhesive sheets so as to realize the wavelength conversion of the LED emergent light. Although such packaging forms are improved in terms of operation convenience, cost and the like compared with the conventional technology, there are drawbacks such as adverse heat transfer generated during the operation of the LED, and this problem has a great influence on the performance of the LED. On the other hand, the conventional radiator structure is still adopted in the existing LED radiating technology, and heat is radiated through heat conduction, but the radiating performance of the LED radiating technology is still to be further improved, so that the service life of the LED is prolonged. The organic silicon packaging material has excellent thermal stability, water resistance and light transmittance because the organic silicon packaging material has the structure of both organic groups and inorganic groups, and the organic silicon packaging material continuously replaces the traditional packaging material and becomes an important research direction of the LED packaging material at home and abroad.
However, the hardness of the silica gel is relatively low, the surface of the package body is easy to scratch, and the operation performance of the thimble is poor due to easy deformation and warping, so that the hardness of the package body needs to be improved. Therefore, it is important to develop a small particle solid fluorescent glue film with high hardness and easy suction.
Disclosure of Invention
Aiming at the technical problems, the invention provides a preparation method of a double-layer small-particle solid-state fluorescent adhesive film with high hardness and low warpage, which comprises the following steps:
step one: a fluorescent adhesive film is coated on the release film in a scraping way;
step two: a transparent adhesive film is coated on the release film in a scraping way;
step three: the fluorescent adhesive film and the transparent adhesive film are compositely overlapped by using a vacuum lamination machine;
step four: the resulting material was cured at temperature and then cut.
As a preferable technical scheme, the thickness of the fluorescent glue film is 30-70 mu m.
As a preferred technical scheme, the fluorescent glue film is a silicone resin semi-cured prepolymer, and the rheological property of the fluorescent glue film needs to meet the viscosity of 5000-10000 Pa.s.
As a preferable technical scheme, the fluorescent adhesive film is prepared from the following raw materials in parts by mass: 20-99 parts of organic silicon resin and 1-80 parts of fluorescent powder.
As a preferable technical scheme, the thickness of the transparent adhesive film is 30-80 mu m.
As a preferable technical scheme, the storage modulus G' of the transparent coating film is 20-2000KPa, and the loss modulus is 30-900KPa.
As a preferable technical scheme, the transparent adhesive film is prepared from the following raw materials in parts by mass: 20-50 parts of high refractive index organic silicon resin and 50-80 parts of micron-sized inorganic filler.
As a preferable technical scheme, the micron-sized inorganic filler has a particle size of 1-70 μm.
As a preferred technical scheme, the viscosity of the high-refractive-index silicone resin is 5000-70000 Pa.s.
As a preferable technical scheme, the refractive index of the high refractive index silicone resin is 1.50-1.60.
Advantageous effects
The invention provides a manufacturing method of a high-hardness low-warpage double-layer small-particle solid-state fluorescent adhesive film, which comprises a double-layer structure: the inner layer is a fluorescent glue film containing fluorescent powder and having the thickness of 30-70 um; the outer layer is a transparent adhesive film with the thickness of 30-80um and containing 50-80% of inorganic filler by weight. The heat generated by the inner layer ultrathin structure is low and is easier to be conducted to the substrate for heat dissipation, and the outer layer adhesive film is added with the high-content micron-sized filler to give out excellent heat resistance, so that the whole packaging structure has good heat resistance and can be used for high-power devices. The micron-sized filler in the outer adhesive film effectively improves the hardness of the outer adhesive film, so that the cut double-layer adhesive film small particles have high enough hardness, and the customer ejector pin sucking operation is easy. By adding the high-content micron-sized inorganic filler, the hardness of the organic silica gel mold is increased, the transparency of the product is ensured, and meanwhile, the moisture resistance of the product can be increased.
Drawings
FIG. one is a schematic diagram of a dual-layer small particle phosphor film according to the present invention.
Wherein: 1. a nano inorganic filler; 2. transparent adhesive tape; 3. fluorescent powder; 4. and (5) a fluorescent adhesive film.
Detailed Description
The technical features of the technical solution provided in the present invention will be further clearly and completely described in connection with the detailed description below, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The words "preferred," "more preferred," and the like in the present disclosure refer to embodiments of the present disclosure that may provide certain benefits in some instances. However, other embodiments may be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
The invention provides a preparation method of a double-layer small-particle solid-state fluorescent adhesive film with high hardness and low warpage, which comprises the following steps:
step one: a fluorescent adhesive film is coated on the release film in a scraping way;
step two: a transparent adhesive film is coated on the release film in a scraping way;
step three: the fluorescent adhesive film and the transparent adhesive film are compositely overlapped by using a vacuum lamination machine;
step four: and (5) carrying out cutting after curing the obtained material at high temperature.
[ fluorescent glue film ]]
The fluorescent adhesive film prepared by the method is an organosilicon resin semi-cured prepolymer. In some embodiments, the phosphor film has a thickness of 30-70 μm.
Preferably, the fluorescent glue film comprises the following preparation raw materials in parts by weight: 20-99 parts of organic silicon resin and 1-80 parts of fluorescent powder.
Furthermore, the raw materials for preparing the fluorescent glue film also comprise auxiliary agents such as an anti-settling agent and the like.
< phosphor powder >
Preferably, the particle size of the phosphor is 1 to 70 μm.
Further preferably, the particle size of the phosphor is 10 to 15. Mu.m.
Preferably, the fluorescent glue film contains 5-80wt% of fluorescent powder
The fluorescent powder comprises any one or more of rare earth fluorescent powder, rare earth garnet fluorescent powder, alkaline earth metal gallium sulfide, alkaline earth metal sulfide, zinc sulfide, alkaline earth metal aluminate, phosphate, borate, silicate, fluorine arsenate, fluorine germanate, rare earth sulfide, rare earth oxide, vanadate and nitride fluorescent powder. Preferably, the fluorescent powder can be aluminate, silicate, nitride and oxynitride fluorescent powder with better chemical and high-temperature stability, in particular nitride and oxynitride fluorescent powder. Preferably, the fluorescent powder is rare earth element doped YAG yttrium aluminum garnet fluorescent powder or Ce doped YAG yttrium aluminum garnet fluorescent powder.
Preferably, the phosphor in the present invention is at least one of YAG phosphor, nitride phosphor, and silicate phosphor.
YAG 538 fluorescent powder (Hongda trade company, inc.) and YH-Y538M, YH-Y558M, YH-Y565M, respectively, are YAG-01, YAG-02, YAG-1A, YAG-2A, YAG-04, YAG-05 and YAG-06 fluorescent powders.
The nitride fluorescent powder is MPR-1003/D fluorescent powder (Mitsubishi chemical (China) commercial and trade company, inc.), YH-C625E fluorescent powder (Hangzhou fluorescent crane photoelectric material Co., ltd.), YH-C630E and YH-C630 fluorescent powder (Hangzhou fluorescent crane photoelectric material Co., ltd.), the Dino series (DINO) nitride has the types of M3028A, AM3028, AM3058 fluorescent powder, warm white high color developing single powder and the nitride high color developing red powder has the types of R-610, R-620, R-630, R-640, R-650, R-655 and R-670 fluorescent powder.
The silicate fluorescent powder is G2762-10 fluorescent powder (Lanbo photoelectric (Suzhou) technology Co., ltd.), G2762-15 (Lanbo photoelectric (Suzhou) technology Co., ltd.), and the German merck silicate fluorescent powder is SGA515-100, SGA521-100, SGA530-100, SGA540-100, SGA550-100, SGA560-100, SGA580-100, SGA600-100 or SGA605-100 fluorescent powder.
Further preferably, the fluorescent powder is Intermet YAG-05.
The sources of the phosphors described in the present invention are not limited and may be prepared by methods well known to those skilled in the art or commercially available.
< Silicone resin >
The organic silicon resin in the raw materials for preparing the fluorescent glue film is not particularly limited, and various organic silicon resins well known to those skilled in the art can be selected.
Further preferably, the silicone resin of the fluorescent glue film prepared by the invention is DuPont LF-1112A/B.
In some embodiments, the method for preparing the fluorescent glue film comprises the following steps: and (3) processing 20-99 parts of silicone resin and 1-80 parts of fluorescent powder by a stirrer and a kneader to obtain a mixture 2, and extruding and coating or calendaring the mixture 2 onto a release film to form a fluorescent adhesive film with uniform thickness of 30-70 um.
In some embodiments, the phosphor film made according to the method described above is a silicone semi-cured prepolymer having a rheology that meets the viscosity of 6000-8000 Pa.s, a test temperature of 60 ℃, and a rotor spin speed of 8RPM.
[ transparent adhesive film ]]
In the invention, the transparent adhesive film comprises the following raw materials in parts by weight: 20-50 parts of organic silicon resin and 50-80 parts of micron-sized inorganic filler.
In some embodiments, the raw material of the transparent adhesive film further comprises an anti-settling agent.
Preferably, the thickness of the transparent adhesive film is 30-80 mu m.
< micron-sized inorganic filler >
In the present invention, the specific components and types of the micron-sized inorganic filler are not particularly limited, and various components known to those skilled in the art may be selected, including but not limited to any one or more of titanium dioxide, zirconium dioxide, silicon oxide, boron nitride, zinc oxide, aluminum oxide, magnesium oxide, mica, rare earth metal oxide. The micron-sized inorganic filler of the present invention may also be prepared by conventional means in the art or commercially available.
In some embodiments, the microscale inorganic filler is added in an amount of 50-80wt%.
Further preferably, the addition amount of the micron-sized inorganic filler is 50-70wt%.
The inventor finds that when the addition amount of the micron-sized inorganic filler is less than 50%, the effect of the micron-sized inorganic filler on improving the hardness is not obvious, and the sucking operation of a customer is difficult to meet; and when the addition amount is higher than 70%, the viscosity of the whole organic silicon system is too high (> 80000 mPa.s), and the prefabricated film forming is difficult. Meanwhile, the addition amount of the micron-sized inorganic filler can increase the hardness of the organic silica gel film to Shore D75-Shore D90 when 50-70wt%, can prevent the surface of the adhesive film from being scratched, and has the advantages of easy suction, no warpage and the like.
The nanoscale inorganic filler particles can increase the thermal conductivity and the light attenuation resistance of the transparent adhesive film.
In some embodiments, the nanoscale inorganic filler has a particle size of 0.001 μm to 500 μm.
Further preferably, the nanoscale inorganic filler has a particle diameter of 1 μm to 70 μm,
more preferably, the nanoscale inorganic filler has a particle size of 10 μm to 15. Mu.m.
The inventor finds that when the particle size is too large, the surface of the prefabricated adhesive film is raised by the large particles of the fluorescent powder, and the surface of the adhesive film is not smooth after being packaged into the double-layer small particles, so that the consistency of color temperature is seriously affected; when the particle size is too small, the effect on the performance such as hardness increase, moisture resistance, heat resistance and the like is not obvious.
Preferably, the general formula of the micron-sized inorganic filler may be expressed as:
M(1-x-y-z-u)+vA x B y C z D u E v o0.5 (1+x+2y+3z+3u), wherein m=na, K; a= Mg, ca, sr, zn; b=b, al, ga; c=si, ge, sn; d=zr, ti; e= F, cl. For the content of each element, x is specified<0.3；0.1<y<0.3；0.4<z<0.7；u<0.3；v<0.1, and x+y+z+u-v>0.1。
< Silicone resin >
In the present invention, the silicone resin has a main chain formed mainly of siloxane bonds (-si—o—si-) and a side chain formed of an organic group such as an alkyl group (e.g., methyl group or the like), an aryl group (e.g., phenyl group or the like), or an alkoxy group (e.g., methoxy group) bonded to a silicon atom (Si) of the main chain in a molecule. Specifically, examples of the silicone resin composition include a dehydration condensation curable silicone resin, an addition reaction curable silicone resin, a peroxide curable silicone resin, a moisture curable silicone resin, and other curable silicone resins. The resins may be used singly or in combination of two or more.
In some preferred embodiments, the silicone resin employed in the transparent adhesive film of the present invention is a high refractive index silicone encapsulation resin.
Preferably, the silicone resin has a refractive index of 1.40-1.70.
Preferably, the silicone resin has a viscosity of 5000-7000mpa.s.
Further preferably, the organosilicon resin of the transparent adhesive film is Dow Corning OE-6650A/B. Further preferably, the weight ratio between the A and B components of OE-6650 is 1:3 (viscosity 6000cP after mixing).
The high refractive index silicone encapsulation resin of the present invention may also be prepared by methods well known to those skilled in the art, for example, the preparation method thereof includes the steps of: uniformly stirring 55-75 parts by mass of vinyl phenyl polysiloxane and 25-45 parts by mass of vinyl phenyl silicone oil; adding 3.0X10-4-1.5X10-3 parts of card platinum catalyst, and stirring; the component B is prepared by the following method: uniformly stirring 30-40 parts of hydrogen-containing phenyl polysiloxane, 9-12 parts of heptamethyl trisiloxane and 45-60 parts of phenyl vinyl polysiloxane containing epoxy groups according to mass; adding 0.05-0.1 part of inhibitor and 1-3 parts of tackifier, and stirring uniformly. Wherein the epoxy-based styrene and tackifier can be prepared by a conventional method.
In some embodiments, the second operation is to process 20-50 parts of silicone resin and 50-80 parts of micron-sized inorganic filler by a stirrer and a kneader to obtain a mixture 1, and then extrusion-coat or calender the mixture 1 onto a release film to form a silicone transparent adhesive film with a thickness of 30-80um and a uniform thickness.
The transparent adhesive film prepared by the method is a hot-melt material, and has the following rheological properties: the TA DHR rheometer is used for testing the vertebral plate with the diameter D=25 mm, the oscillation frequency is 1Hz, the strain is 0.1%, the testing temperature range is 25-150 ℃, the heating rate is 5 ℃/min, the storage modulus G' value is 20-2000KPa, the loss modulus is 30-900KPa, and the gel point is 6-8min.
The specific components of the anti-settling agent in the raw materials of the fluorescent adhesive film and the transparent adhesive film are not particularly limited, and various anti-settling agent components known to those skilled in the art can be selected, including but not limited to Yu Deshan chemical DM-30.
[ Compound film ]]
The material of the release film in the invention comprises one of PET, PP, PE, and no special requirement is required.
Preferably, the release film is PET.
Preferably, the step three is to peel off the PET film, the fluorescent adhesive film and the transparent adhesive film, and then the fluorescent adhesive film and the organic silicon transparent adhesive film containing the micron-sized inorganic filler are pressed together through a vacuum laminating machine to prepare the double-layer film material.
Preferably, the step four is to fully solidify the obtained double-layer film material at the high temperature of 150-200 ℃ in an air drying box, and then cut the double-layer film material by a cutting machine without water or with water to obtain the double-layer small-particle solid fluorescent glue.
The present invention will be specifically described below by way of examples. It is noted herein that the following examples are given solely for the purpose of further illustration and are not to be construed as limitations on the scope of the invention, as will be apparent to those skilled in the art in light of the foregoing disclosure.
Examples 1-5 provide a method for producing a silicone transparent adhesive film containing a micron-sized inorganic filler, comprising the steps of:
1. taking organic silicon packaging resin according to the mass ratio, and treating the LF-158 grade inorganic filler with the particle size of 12 mu m by a stirrer and a kneader to obtain a mixture 1;
2. the mixture 1 was extrusion coated or calendered onto a release film to form a silicone transparent adhesive film having a thickness of 80 μm and a uniform thickness.
The organic silicon packaging resin is OE-6650A/B, DM-30 and 12 μm micron-sized inorganic filler, and the release film is PET.
Example 1 provides a method for manufacturing an organosilicon transparent adhesive film containing micron-sized inorganic filler, wherein the micron-sized inorganic filler is 0wt% and the DM-30 content is 1wt%.
Example 2 provides a method for manufacturing an organosilicon transparent glue film containing micron-sized inorganic filler, wherein the micron-sized inorganic filler is 50wt% and the DM-30 content is 1wt%.
Example 3 provides a method for manufacturing an organosilicon transparent glue film containing micron-sized inorganic filler, wherein the micron-sized inorganic filler is 60wt% and the DM-30 content is 1wt%.
Example 4 provides a method for manufacturing a silicone transparent adhesive film containing micron-sized inorganic filler, wherein the micron-sized inorganic filler is 70wt% and the DM-30 content is 1wt%.
Example 5 provides a method for manufacturing a silicone transparent adhesive film containing a micron-sized inorganic filler, wherein the micron-sized inorganic filler is 80wt% and the DM-30 content is 1wt%.
The applicant carried out the water absorption test, hardness test and thermal resistance test on the organosilicon transparent adhesive film containing the micron-sized inorganic filler in the above examples.
The water absorption test method comprises the following steps: cutting the prefabricated transparent adhesive film with the thickness of 80 mu M and containing the micron-sized inorganic fillers with different addition amounts into strips with the thickness of 50mm to 20mm, and weighing M 0 Soaking in boiling water, decocting for 1 hr, taking out, sucking the surface water of the adhesive film with dust-free paper, and weighing M 1 Then the water absorption rate is obtained by taking the formula I.
Equation one: boiling water absorption= (M 1 -M 0 )/M0*100％
The hardness testing method comprises the following steps: the hardness test is carried out on the prefabricated transparent adhesive film with the thickness of 80 mu m and containing the micron-sized inorganic fillers with different addition amounts, and the hardness test equipment is Shore D digital display Shore hardness tester, shanghai Shuangxu electronic Co.
The thermal resistance test method comprises the following steps: the hardness test is carried out on prefabricated transparent adhesive films with the thickness of 80 mu m and containing different addition amounts of micron-sized inorganic fillers, and the test equipment is a T3Ster thermal resistance tester of Shenzhen Michaen technology Co.
The test results of the samples in the above examples are shown in table 1 below:
table A test result of the performance of the transparent adhesive film with the thickness of 80 μm containing the micron-sized inorganic fillers with different addition amounts
| Scheme for the production of a semiconductor device | Boiling water uptake (%) 100 ℃/1 hour | Hardness Shore D | Thermal resistance rate of W |
| Example 1 | 0.104 | 69 | 4.511 |
| Example 2 | 0.040 | 77 | 3.814 |
| Example 3 | 0.036 | 80 | 3.814 |
| Example 4 | 0.030 | 85 | 3.243 |
| Example 5 | 0.021 | 91 | 2.511 |
The test result shows that the adhesive film without adding the micron-sized inorganic filler has the largest boiling water absorption rate, the adhesive film with adding the micron-sized inorganic filler has the boiling water absorption rate reduced along with the increase of the content of the filler, the hardness is increased along with the increase of the adding amount of the micron-sized inorganic filler, and the larger the adding amount of the micron-sized inorganic filler in the outermost transparent layer is, the lower the thermal resistance is, namely the better the heat conducting property of the product is.
Example 6 the present invention provides a method for manufacturing a double-layer small particle solid state fluorescent glue film easy to have high hardness and low warpage, the manufacturing method comprises the following steps:
step one: 20 parts of LF-1112A glue, 20 parts of LF-1112B glue, 20 parts of YAG 04 fluorescent powder with the particle size of 12 mu m and 20 parts of YAG 05 fluorescent powder with the particle size of 12 mu m are processed by a stirrer and a kneader to obtain a mixture 2, and the mixture 2 is extruded and coated on a PET film to form a fluorescent glue film with the thickness of 60 mu m uniformly.
Step two: and (3) carrying out treatment on 19 parts of OE-6650A/B, 1 part of DM-30 parts of LF-158 micron-sized inorganic filler with the particle size of 12 mu m and 80 parts of LF-158 micron-sized inorganic filler by a stirrer and a kneader to obtain a mixture 1, and extruding and coating the mixture 1 on a PET film to form the organosilicon transparent adhesive film with the thickness of 80 mu m and uniform thickness.
Step three: and pressing the fluorescent adhesive film and the organic silicon transparent adhesive film containing the micron-sized inorganic filler by a vacuum laminating machine to prepare the double-layer film material.
Step four: and (3) fully curing the obtained double-layer film material at the high temperature of 200 ℃ in an air drying box, and then cutting with water by a cutting machine to obtain the double-layer small-particle solid fluorescent glue.
The vacuum laminating machine is VHP-200, the forced air drying oven is DHG-9070A, and the precise scribing cutter is DS613.
Example 7 the present invention provides a method for manufacturing a high-hardness low-warpage double-layer small-particle solid-state fluorescent film, comprising the following steps:
step one: 20 parts of LF-1112A glue, 20 parts of LF-1112B glue, 20 parts of YAG 04 fluorescent powder with the particle size of 12 mu m and 20 parts of YAG 05 fluorescent powder with the particle size of 12 mu m are processed by a stirrer and a kneader to obtain a mixture 2, and the mixture 2 is extruded and coated on a PET film to form a fluorescent glue film with the thickness of 60 mu m uniformly.
Step two: and (3) carrying out treatment on 19 parts of OE-6650A/B, 1 part of DM-30 parts of LF-158 micron-sized inorganic filler with the particle size of 12 mu m and 80 parts of LF-158 micron-sized inorganic filler by a stirrer and a kneader to obtain a mixture 1, and extruding and coating the mixture 1 on a PET film to form the organosilicon transparent adhesive film with uniform thickness.
Step three: and pressing the fluorescent adhesive film and the organic silicon transparent adhesive film containing the micron-sized inorganic filler by a vacuum laminating machine to prepare the double-layer film material.
Step four: and (3) fully curing the obtained double-layer film material at the high temperature of 200 ℃ in an air drying box, and then cutting with water by a cutting machine to obtain the double-layer small-particle solid fluorescent glue.
The vacuum laminating machine is VHP-200, the forced air drying oven is DHG-9070A, and the precise scribing cutter is DS613.
Example 8 the present invention provides a method for manufacturing a high-hardness low-warpage double-layer small-particle solid-state fluorescent film, which comprises the following steps:
step one: and (3) processing 20 parts of LF-1112A glue, 20 parts of LF-1112B glue, 20 parts of YAG 04 fluorescent powder with the particle size of 12 mu m and 20 parts of YAG 05 fluorescent powder with the particle size of 12 mu m by a stirrer and a kneader to obtain a mixture 2, and extruding and coating the mixture 2 onto a PET separating film to form a fluorescent glue film with uniform thickness.
Step two: and (3) carrying out treatment on 19 parts of OE-6650A/B, 1 part of DM-30 parts of LF-158 micron-sized inorganic filler with the particle size of 80 mu m and 80 parts of LF-158 micron-sized inorganic filler by a stirrer and a kneader to obtain a mixture 1, and extruding and coating the mixture 1 onto a PET film to form the organosilicon transparent adhesive film with uniform thickness.
Step three: and pressing the fluorescent adhesive film and the organic silicon transparent adhesive film containing the micron-sized inorganic filler by a vacuum laminating machine to prepare the double-layer film material.
Step four: and (3) fully curing the obtained double-layer film material at the high temperature of 200 ℃ in an air drying box, and then cutting with water by a cutting machine to obtain the double-layer small-particle solid fluorescent glue.
The vacuum laminating machine is VHP-200, the forced air drying oven is DHG-9070A, and the precise scribing cutter is DS613.
Example 9 the present invention provides a method for manufacturing a double-layer small particle solid state fluorescent glue film which is easy to have high hardness and low warpage, comprising the following steps:
step one: and (3) processing 20 parts of LF-1112A glue, 20 parts of LF-1112B glue, 20 parts of YAG 04 fluorescent powder with the particle size of 80 mu m and 20 parts of YAG 05 fluorescent powder with the particle size of 4 mu m5 by a stirrer and a kneader to obtain a mixture 2, and extruding and coating the mixture 2 onto a PET film to form a fluorescent glue film with the thickness of 60 mu m uniformly.
Step two: and (3) carrying out treatment on 19 parts of OE-6650A/B, 1 part of DM-30 parts of LF-158 micron-sized inorganic filler with the particle size of 12 mu m and 80 parts of LF-158 micron-sized inorganic filler by a stirrer and a kneader to obtain a mixture 1, and carrying out extrusion coating on the mixture 1 on a PET film to form the organic silicon transparent adhesive film with the thickness of 80 mu m and uniform thickness.
Step three: and pressing the fluorescent adhesive film and the organic silicon transparent adhesive film containing the micron-sized inorganic filler by a vacuum laminating machine to prepare the double-layer film material.
Step four: and (3) fully curing the obtained double-layer film material at the high temperature of 200 ℃ in an air drying box, and then cutting with water by a cutting machine to obtain the double-layer small-particle solid fluorescent glue.
The vacuum laminating machine is VHP-200, the forced air drying oven is DHG-9070A, and the precise scribing cutter is DS613.
The applicant carried out an optical performance test on the manufacturing method of the double-layer small-particle solid-state fluorescent film with high hardness and low warpage of the above-mentioned examples 6 to 9.
The wafers used for the optical performance were 55X 55mil, the lighting voltage was 3V, and the CIE X and CIE Y variation values DeltaX and DeltaY were less than 4% in the current 1500mA test results. After the packaging glue layer is lightened for 1000 hours, the packaging glue layer is placed in red ink at the temperature of 100 ℃ for 2 hours, then whether the red ink permeates into the packaging glue layer is observed, and if yes, the performance is poor; if not, the performance is good.
The CIE X and CIE Y variation values DeltaX and DeltaY of examples 6-9 are less than 4% per mill, as shown in Table 2 below:
TABLE 2
| Lighting time/hour | DeltaX (variation of CIE X) | Delta Y (variation of CIE Y) |
| 100 | 0.0010 | 0.0030 |
| 200 | 0.0012 | 0.0032 |
| 300 | 0.0015 | 0.0034 |
| 400 | 0.0019 | 0.0036 |
| 500 | 0.0025 | 0.0038 |
| 600 | 0.0023 | 0.0036 |
| 700 | 0.0027 | 0.0039 |
| 800 | 0.0029 | 0.0041 |
| 900 | 0.0031 | 0.0042 |
| 1000 | 0.0029 | 0.0039 |
TABLE 3 results of optical Property tests for examples 6-9
The application relates to a fluorescent adhesive film in the field of semiconductors, in particular to a preparation method of a double-layer small-particle solid fluorescent adhesive film with high hardness and low warpage. The inner layer is a fluorescent adhesive film containing fluorescent powder and having a thickness of 30-70 mu m, and the outer layer is a transparent adhesive film containing 50-80wt% of inorganic filler and having a thickness of 30-80 mu m. The double-layer small-particle solid-state fluorescent adhesive film prepared by the method has good optical performance, high hardness (Shore D80-Shore D90), scratch resistance, no deformation and no warpage, and excellent heat conduction and light attenuation resistance, and can be used for high-power (4.5W) LED devices.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to equivalent embodiments without departing from the technical content of the present invention, and any simple modification, equivalent changes and modification to the above embodiments according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (1)
1. The preparation method of the double-layer small-particle solid-state fluorescent adhesive film with high hardness and low warpage is characterized by comprising the following steps of:
step one: 20 parts of LF-1112A glue, 20 parts of LF-1112B glue, 20 parts of YAG 04 fluorescent powder with the particle size of 12 mu m and 20 parts of YAG 05 fluorescent powder with the particle size of 12 mu m are processed by a stirrer and a kneader to obtain a mixture 2, and the mixture 2 is extruded and coated on a PET film to form a fluorescent glue film with the thickness of 60 mu m uniformly;
step two: 19 parts of OE-6650A/B, 1 part of DM-30 parts of LF-158 micron-sized inorganic filler with the particle size of 12 mu m and 80 parts of LF-158 micron-sized inorganic filler are treated by a stirrer and a kneader to obtain a mixture 1, and the mixture 1 is extruded and coated on a PET film to form an organosilicon transparent adhesive film with the thickness of 80 mu m and uniform thickness;
step three: the fluorescent adhesive film and the organic silicon transparent adhesive film containing the micron-sized inorganic filler are pressed by a vacuum laminating machine to prepare a double-layer film material;
step four: fully curing the obtained double-layer film material at the high temperature of 200 ℃ in an air drying box, and then cutting with water by a cutting machine to obtain double-layer small-particle solid fluorescent glue;
the vacuum laminating machine is VHP-200, the forced air drying oven is DHG-9070A, and the precise scribing cutter is DS613.
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