CN111635723B - Single-component dam material composition and preparation method thereof - Google Patents
Single-component dam material composition and preparation method thereof Download PDFInfo
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- CN111635723B CN111635723B CN202010515246.8A CN202010515246A CN111635723B CN 111635723 B CN111635723 B CN 111635723B CN 202010515246 A CN202010515246 A CN 202010515246A CN 111635723 B CN111635723 B CN 111635723B
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
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- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Epoxy Resins (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a single-component dam material composition and a preparation method thereof, wherein the single-component dam material composition comprises the following components: 5-20 parts by mass of epoxy resin, 5-20 parts by mass of curing agent, 0.1-5 parts by mass of curing accelerator, 55-90 parts by mass of inorganic filler, 0.3-10 parts by mass of fumed silica and 0.3-10 parts by mass of organically modified bentonite; wherein, the epoxy resin adopts one or more of aminophenol trifunctional epoxy resin or tetrafunctional aliphatic epoxy resin. According to the invention, through the combination of the aminophenol trifunctional epoxy resin or the tetrafunctional aliphatic epoxy resin, the fumed silica and the organic modified bentonite, the height-diameter ratio and the thixotropy are obviously improved, the viscosity under high shear force is maintained, the sizing is easy, and the dam material cannot collapse and diffuse during sizing and heating curing.
Description
Technical Field
The invention belongs to the field of semiconductor chip packaging materials, and particularly relates to a single-component dam material composition and a preparation method thereof.
Background
The dam material is used for sealing a semiconductor chip having a multilayer structure manufactured by FC (Flip chip) mounting, TSV (Through Silicon Via) connection, or the like, and can be molded on a substrate or a wafer at a high height-to-diameter ratio, dam a region to be filled, effectively control a filling range of a filling paste, completely fill gaps between elements without allowing a bottom filler to overflow from the substrate or the wafer, and form a cured product having high adhesion to the bottom filler and toughness.
The current dam materials generally have the problems that colloid collapses and diffuses when the glue is applied and heated.
Disclosure of Invention
The invention aims to provide a single-component dam material composition which can not collapse and diffuse when glue is applied and heated and a preparation method thereof.
The invention provides a single-component dam material composition, which comprises the following components:
the epoxy resin is one or more of aminophenol trifunctional epoxy resin or tetrafunctional aliphatic epoxy resin.
Further, the single-component dam material composition further comprises a coloring agent, wherein the coloring agent is 0-5 parts by mass, and the mass part is not 0.
Further, the epoxy resin is one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, biphenyl type epoxy resin, aminophenol trifunctional epoxy resin and tetrafunctional aliphatic epoxy resin, preferably one or more of aminophenol trifunctional epoxy resin and tetrafunctional aliphatic epoxy resin.
Furthermore, the curing agent adopts one or more of modified amine, thiol, acid anhydride and phenolic resin curing agents.
Furthermore, imidazole curing accelerator is adopted as the curing accelerator.
Further, the inorganic filler is one or more of spherical fused silica, crystalline silica, alumina, boron nitride, aluminum nitride, silicon nitride, magnesium oxide, and magnesium silicate.
Furthermore, the organic modified bentonite adopts quaternary ammonium salt modified bentonite.
The preparation method of the single-component dam material composition provided by the invention comprises the following steps:
mixing epoxy resin, a curing agent, a curing accelerator, inorganic filler, fumed silica and organic modified bentonite according to parts by mass;
grinding the obtained mixture on three rollers to obtain paste;
and (4) defoaming the paste in vacuum.
Compared with the prior art, the invention has the following beneficial effects:
the traditional dam material generally has the problems of poor shape maintenance performance, poor thixotropy and collapse and diffusion during sizing and heating curing (60-130 ℃). According to the invention, through the combination of the aminophenol trifunctional epoxy resin (or tetrafunctional aliphatic epoxy resin), the fumed silica and the organic modified bentonite, the height-diameter ratio and the thixotropy are obviously improved, the viscosity under high shear force is maintained, the sizing is easy, and the dam material cannot collapse and diffuse during sizing and heating curing (60-130 ℃).
Detailed Description
The single-component dam material composition comprises 5-20 parts by mass of epoxy resin, 5-20 parts by mass of curing agent, 0.1-5 parts by mass of curing accelerator, 55-90 parts by mass of inorganic filler, 0.3-10 parts by mass of fumed silica and 0.3-10 parts by mass of organically modified bentonite; if necessary, a colorant such as carbon black may be included. Wherein, the weight part of the curing agent is preferably 5 to 10, and the weight parts of the fumed silica and the organic modified bentonite are preferably 0.3 to 3.
The epoxy resin is used as a main resin, and generally one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, biphenyl type epoxy resin, aminophenol trifunctional epoxy resin and tetrafunctional aliphatic epoxy resin can be selected, and one or more of aminophenol trifunctional epoxy resin and tetrafunctional aliphatic epoxy resin is preferably selected. The chemical structural formula of the aminophenol trifunctional epoxy resin is shown in the specification
The aminophenol trifunctional epoxy resin can be specifically MY0510 trifunctional epoxy resin or AFG-90H high-performance trifunctional epoxy resin. The chemical structural formula of the tetrafunctional aliphatic epoxy resin is shown in the specification
The tetrafunctional aliphatic epoxy resin can be PETG epoxy resin.
The curing agent can be one or more of modified amine, thiol, acid anhydride and phenolic resin curing agents according to requirements. The chemical structural formula of the modified amine curing agent is
Wherein R is1～R3Independent of each otherIs selected from a hydrocarbon group having 1 to 6 carbon atoms, namely R1、R2、R3Selected from alkyl with 1-6 carbon atoms, R1、R2、R3Identical, partially identical or completely different. The chemical structural formula of the thiol curing agent is shown in the specification
The curing accelerator adopts imidazole curing accelerator.
The inorganic filler is selected from known inorganic fillers such as spherical fused silica, crystalline silica, alumina, boron nitride, aluminum nitride, silicon nitride, magnesium oxide, magnesium silicate, and the like.
The fumed silica and the organic modified bentonite are cooperatively used as a thixotropic agent for regulating the thixotropy of resin extraction system. The organic modified bentonite is sheet silicate modified with organic matter, and may be modified with quaternary ammonium salt, such as GARAMITE-1958 bentonite. The organic modified bentonite is prepared by using natural bentonite as a raw material, utilizing the lamellar structure of montmorillonite in the bentonite and the characteristic that the lamellar structure can be swelled and dispersed into colloidal clay in water or an organic solvent, and inserting an organic covering agent into the lamellar structure by an ion exchange technology. The quaternary ammonium salt type cationic modifier is a commonly used bentonite organic modifier.
The organically modified bentonite is composed of a sheet-shaped structure and a rod-shaped structure, and the bentonite with different forms can promote the space of the particle sheet layer to be enlarged and become easy to disperse. After dispersion, the edges form hydrogen bonds with each other, and the rod-like and sheet-like shapes "support" each other. The multi-branched epoxy resin combined with three functional groups (four functional groups) forms a net structure by intermolecular force, and the two structures are favorable for forming more free spaces and show strong shear thinning in a macroscopic view. And the fumed silica can improve the medium-low shear viscosity in the system due to the formation of hydrogen bonds and generate a thixotropic phenomenon. Because of the characteristics of serious insufficient coordination, huge specific surface area, surface oxygen deficiency and the like on the surface, the modified organic silicon dioxide modified organic bentonite has strong activity, can easily perform bonding action with oxygen of multi-branched epoxy cyclic molecules, improves the intermolecular bonding force, and has high flow ripple performance because a part of fumed silica particles are still distributed in gaps of macromolecular chains of the organic modified bentonite and the epoxy resin.
In the present invention, although the addition of fumed silica can increase the thixotropy, the viscosity under shear force is also increased, and sizing is difficult. The multi-branched epoxy resin with three functional groups (four functional groups), the fumed silica and the organic modified bentonite have synergistic effect, so that the thixotropy of the dam material can be improved, the viscosity under high shear force can be maintained, and the glue is easy to apply.
In order to make the objects, technical solutions and advantages of the present invention more clearly apparent, the technical effects of the present invention will be further described in detail below with reference to examples and comparative examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The formulations of the examples and comparative examples are shown in Table 1, and the following performance tests were performed for examples 1 to 6 and comparative examples 1 to 3.
(1) Viscosity at room temperature: the viscosity of the adhesive was measured at 5rpm using a Brookfield viscometer using a 14# spindle
(2) Thixotropic index: the viscosity of the adhesive was tested with a Brookfield viscometer using a 14# spindle at 5rpm for V1 and at 0.5rpm for V2, thixotropic index, V2/V1.
(3) Height-diameter ratio: the ratio of the height (h) to the width (d) of the cured dispensing glue solution is defined as the height-diameter ratio and is used as an index of the shape maintaining performance of the dam material composition.
(4) Whether or not to collapse and spread when sizing: the glue solution is spotted on a glass plate, the fixed width is 0.6mm, the glue applying height is tested, whether the glue solution collapses and diffuses during glue applying is observed,
(5) whether collapse and diffusion occurs during heat curing: and (3) putting the glue solution after gluing into a drying oven for heating and curing, and observing whether the glue solution collapses and diffuses.
TABLE 1 example and comparative example formulations and Performance evaluation
As can be seen from table 1, the dam using only fumed silica or organically modified bentonite has a low aspect ratio, poor thixotropy, and collapse and diffusion of the colloid during sizing and heating. The combination of fumed silica and organically modified bentonite is adopted, but the epoxy resin is selected from the traditional bisphenol A epoxy resin, the dam material still has low height-diameter ratio and poor thixotropy, and the colloid collapses and diffuses during sizing and heating. However, the combination of aminophenol trifunctional epoxy resin (or tetrafunctional aliphatic epoxy resin), fumed silica and organically modified bentonite is adopted, so that the problems in the comparative example can be obviously improved, the height-diameter ratio and the thixotropy of the dam material are improved, and the colloid does not collapse and diffuse during sizing and heating.
The above embodiments are only for illustrating the technical solutions and technical effects of the present invention, and those skilled in the art can make other variations or modifications based on the above description, and those variations or modifications derived from the spirit of the present invention still fall into the protection scope of the present invention.
Claims (7)
1. The single-component dam material composition is characterized by comprising the following components:
the epoxy resin is one or more of aminophenol trifunctional epoxy resin or tetrafunctional aliphatic epoxy resin.
2. The one-component dam composition of claim 1, wherein:
the color paste also comprises a colorant, wherein the colorant is 0-5 parts by mass, and the mass part does not include an endpoint of 0.
3. The one-component dam composition of claim 1, wherein:
the curing agent is one or more of modified amine curing agents, thiol curing agents, acid anhydride curing agents and phenolic resin curing agents.
4. The one-component dam composition of claim 1, wherein:
the curing accelerator is imidazole curing accelerator.
5. The one-component dam composition of claim 1, wherein:
the inorganic filler is one or more of spherical fused silica, crystalline silica, alumina, boron nitride, aluminum nitride, silicon nitride, magnesium oxide and magnesium silicate.
6. The one-component dam composition of claim 1, wherein:
the organic modified bentonite adopts quaternary ammonium salt modified bentonite.
7. A preparation method of the single-component dam material composition is characterized by comprising the following steps:
mixing epoxy resin, a curing agent, a curing accelerator, an inorganic filler, fumed silica and organically modified bentonite according to the mass part of claim 1;
grinding the obtained mixture on three rollers to obtain paste;
and (4) defoaming the paste in vacuum.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010515246.8A CN111635723B (en) | 2020-06-08 | 2020-06-08 | Single-component dam material composition and preparation method thereof |
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| CN202010515246.8A CN111635723B (en) | 2020-06-08 | 2020-06-08 | Single-component dam material composition and preparation method thereof |
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| CN111635723B true CN111635723B (en) | 2022-03-22 |
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| CN115029045A (en) * | 2022-05-06 | 2022-09-09 | 中国船舶重工集团公司第七二五研究所 | Preparation method of surface defect finishing material of marine environment composite material |
| CN115160965B (en) * | 2022-07-07 | 2023-08-04 | 武汉市三选科技有限公司 | Cofferdam glue and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899195A (en) * | 2009-06-01 | 2010-12-01 | 信越化学工业株式会社 | The manufacture method of dam composition and multi-level semiconductor device |
| CN107652933A (en) * | 2017-10-25 | 2018-02-02 | 绵阳惠利电子材料有限公司 | Magnetic core bonding nanoscale one-component tough epoxy compound and preparation method thereof |
| JP2018097036A (en) * | 2016-12-08 | 2018-06-21 | 株式会社タムラ製作所 | Photosensitive resin composition |
| CN111117540A (en) * | 2019-12-23 | 2020-05-08 | 科化新材料泰州有限公司 | High-strength high-heat-resistance epoxy plastic packaging material for organic bentonite modified semiconductor packaging and preparation method thereof |
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- 2020-06-08 CN CN202010515246.8A patent/CN111635723B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899195A (en) * | 2009-06-01 | 2010-12-01 | 信越化学工业株式会社 | The manufacture method of dam composition and multi-level semiconductor device |
| JP2018097036A (en) * | 2016-12-08 | 2018-06-21 | 株式会社タムラ製作所 | Photosensitive resin composition |
| CN107652933A (en) * | 2017-10-25 | 2018-02-02 | 绵阳惠利电子材料有限公司 | Magnetic core bonding nanoscale one-component tough epoxy compound and preparation method thereof |
| CN111117540A (en) * | 2019-12-23 | 2020-05-08 | 科化新材料泰州有限公司 | High-strength high-heat-resistance epoxy plastic packaging material for organic bentonite modified semiconductor packaging and preparation method thereof |
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