Dispersion liquid, slurry and application thereof

Abstract

The dispersion liquid provided by the embodiment of the invention comprises silicon dioxide modified particles and an organic solvent, and the silicon dioxide modified particles comprise alkoxy silane modified silicon dioxide particles containing aryl. The silicon dioxide modified particles in the dispersion liquid are good in dispersity, the dispersion liquid is high in transparency and good in stability, the dispersion liquid can be mixed with epoxy resin to prepare slurry with high solid content, high dispersion and low viscosity, and the slurry is used for an underfill material so as to improve the service reliability of electronic devices; and the organic silicon material can also be mixed with an organic silicon material to prepare slurry with high solid content, high transparency and low viscosity, and the slurry is used for preparing optical products, so that the optical products have excellent optical properties while having good processability and mechanical properties. The embodiment of the invention further provides slurry containing the dispersion liquid and application of the slurry.

Description

Technical Field

[0001] The embodiments of the present application relate to the technical field of electronic device preparation, and in particular to a dispersion liquid, a slurry and applications thereof. Background Art

[0002] Nano-silicon dioxide is widely used in the field of electronic materials and optoelectronic materials, including integrated circuit packaging materials, photovoltaic materials, LED materials, transistor materials, etc. However, the existing nano-silicon dioxide added to epoxy resin, silicone and other systems often has poor dispersibility, resulting in increased viscosity of the system and affecting the transparency of the original system. In addition, the existing preparation of nano-silicon dioxide may introduce Na + , Cl -1 These impurity ions will corrode metal circuits and have a serious impact on packaging reliability. Summary of the invention

[0003] In view of this, an embodiment of the present application provides a dispersion in which the silica-modified particles have good dispersibility, and the dispersion has high transparency and good stability. The dispersion can be mixed with epoxy resin to prepare a slurry with high solid content, high dispersion and low viscosity, which is used as a bottom filling material to improve the packaging effect.

[0004] Specifically, a first aspect of an embodiment of the present application provides a dispersion, wherein the dispersion comprises silica-modified particles and an organic solvent, wherein the silica-modified particles comprise silica particles modified with alkoxysilane containing an aromatic group.

[0005] The dispersion provided in the embodiment of the present application is a silica dispersion, which contains silica particles modified by alkoxysilane containing an aromatic group. The present application uses alkoxysilane containing an aromatic group to modify the silica particles, which can effectively improve the dispersibility of the silica particles in the dispersion, and improve the stability and transparency of the dispersion. The dispersion can be mixed with epoxy resin to prepare a slurry with high solid content, high dispersion and low viscosity, which is used as a bottom filling material. While obtaining low viscosity and thixotropy, the problem of particle sedimentation can be effectively improved to improve the packaging effect and the reliability of electronic devices. The dispersion can also be mixed with an organic silicon material to prepare a slurry with high solid content, high transparency and low viscosity, which is used for the preparation of optical products, so that the optical products can obtain excellent optical properties while obtaining good processability and mechanical properties.

[0006] In an embodiment of the present application, the number of carbon atoms of the aromatic group-containing alkoxysilane is less than or equal to 18.

[0007] In the embodiment of the present application, the molecular weight of the aromatic alkoxysilane is less than or equal to 600. Controlling the molecular weight of the aromatic alkoxysilane to a smaller value can better control the size of the surface modification group of the modified silica particles, and is also conducive to avoiding the influence of steric hindrance on the modification effect.

[0008] In the embodiment of the present application, in the modified silica particles, the weight proportion of the modified groups derived from the aromatic alkoxysilane is 20%-45%. Controlling the binding amount of the modified groups on the modified silica particles within a suitable range can better improve the dispersibility of the silica particles in the dispersion, and improve the stability and transparency of the dispersion.

[0009] In the embodiment of the present application, the organic solvent includes one or more of N,N-dimethylformamide (DMF), ketone solvents, ester solvents, and benzene solvents. The organic solvent can be selected according to the application needs and system requirements. Among them, the ester solvent can include ethyl acetate, and the benzene solvent can include toluene.

[0010] In the embodiment of the present application, the dispersion does not contain water. The dispersion of the present application does not contain water, which is beneficial to improving the dispersibility of the modified silica particles.

[0011] In the embodiment of the present application, the dispersion does not contain metal ions. In the embodiment of the present application, the dispersion does not contain halogens. In the bottom filling material, the presence of impurity metal ions and halogens will corrode the metal circuits of the chip and have a serious impact on the chip reliability. The silicon dioxide dispersion of the present application does not contain metal ions and halogens. Using it as a filler for the preparation of the bottom filling material can effectively avoid the impact of metal ion impurities and halogen impurities on the reliability of the package.

[0012] In the embodiment of the present application, the particle size D50 of the modified silica particles is 10nm-100nm. Suitable particle size of the modified silica particles is conducive to uniform dispersion in the dispersion liquid, and is also conducive to better complete filling when used as bottom filling material, thereby improving packaging reliability.

[0013] In the embodiment of the present application, the particle size D10 of the modified silica particles is 16nm-35nm, D50 is 20nm-50nm, and D90 is 35nm-60nm. The particle size of silica is relatively uniform and the particle size distribution is narrow, which is conducive to improving the uniformity of the dispersion.

[0014] In the embodiment of the present application, in the dispersion, the particle size distribution coefficient P of the modified silica particles is in the range of 0.07-0.17, wherein P = (D90-D10) / D50. The particle size distribution coefficient of the modified silica particles in this range can better improve the dispersibility of the dispersion.

[0015] In the embodiment of the present application, the dispersion is a monodisperse system. A monodisperse system generally refers to a dispersion system with a single dispersed phase and a narrow particle size distribution, and the particle size distribution is normal distribution or approximately normal distribution.

[0016] In the embodiment of the present application, when the solid content of the dispersion is 35%-50%, the visible light transmittance is 80%-99%. The silicon dioxide dispersion of the embodiment of the present application can effectively improve the dispersibility of the silicon dioxide particles in the dispersion by modifying the silicon dioxide particles with alkoxysilane containing aromatic groups, and improve the transparency of the dispersion, so that it is conducive to application scenarios with high requirements for transparency.

[0017] In the embodiment of the present application, the dispersion liquid uses alkoxysilane as a silicon source and ammonia water as a catalyst to synthesize silica particles in alcohol and water, and then uses the organic solvent for solvent replacement, and uses alkoxysilane containing an aromatic group to modify the silica particles. The dispersion liquid of the present application is prepared by the above process, which can reduce the amount of solvent used, and the reaction conditions are mild. A uniform dispersion effect can be achieved without introducing a dispersant or a dispersant; and the process does not introduce metal ions or halogens, and the dispersion liquid has high purity; the dispersion liquid can be applied to a variety of systems.

[0018] A second aspect of the present invention provides a method for preparing a dispersion, comprising the following steps:

[0019] Alkoxysilane is used as a silicon source and ammonia water is used as a catalyst to obtain a silica particle dispersion by reaction in alcohol and water;

[0020] The silicon dioxide particle dispersion is first subjected to a solvent replacement treatment using an organic solvent, and then the silicon dioxide particles are modified using an alkoxysilane containing an aromatic group to obtain a dispersion; or

[0021] The silica particles in the silica particle dispersion are first modified with an aromatic alkoxysilane, and then a solvent replacement treatment is performed with an organic solvent to obtain a dispersion; the dispersion comprises modified silica particles and the organic solvent, and the modified silica particles comprise silica particles modified with an aromatic alkoxysilane.

[0022] The method for preparing a dispersion provided in an embodiment of the present application adopts a liquid phase method and introduces solvent replacement to obtain a dispersion containing modified silica particles, which can significantly reduce the amount of solvent used, and the reaction conditions of the entire preparation process are mild, and a uniform dispersion effect can be achieved without introducing a dispersant or a dispersant aid; and the preparation process does not introduce metal ions or halogens, and the dispersion has high purity; the dispersion has good dispersibility and high transparency, and can be applied to a variety of systems to meet different application requirements.

[0023] The third aspect of the embodiment of the present application provides the application of the dispersion described in the first aspect or the dispersion prepared by the preparation method described in the second aspect in electronic product manufacturing, optical products, coating materials, functional film materials, adhesives, fillers, medical products, building materials, nanomaterial manufacturing, and environmental protection engineering. In the dispersion of the embodiment of the present application, the silicon dioxide particles have good dispersibility, and the dispersion has high stability and transparency. It can be used as a basic raw material and is suitable for a variety of systems to meet different application requirements.

[0024] A fourth aspect of an embodiment of the present application provides a slurry, which includes an epoxy resin and the silica-modified particles in the dispersion described in the first aspect of the embodiment of the present application or the silica-modified particles in the dispersion prepared by the preparation method described in the second aspect.

[0025] The slurry provided in the embodiment of the present application is an epoxy resin system slurry, which is prepared by mixing the dispersion liquid of the first aspect of the embodiment of the present application with the epoxy resin and removing the organic solvent, and the residual amount of the organic solvent in the obtained slurry is less than 1%. The obtained slurry has the characteristics of high solid content, high dispersion and low viscosity, and is used for bottom filling materials. While obtaining low viscosity and low thixotropy, it can effectively improve the problem of particle sedimentation, improve the packaging effect, and improve the reliability of electronic devices.

[0026] In the embodiment of the present application, the room temperature viscosity of the slurry is lower than 30 Pa·s, and the viscosity at 110°C is lower than 0.075 Pa·s. The slurry has a relatively low viscosity at both room temperature and 110°C, which is conducive to ensuring that the slurry has good fluidity and filling properties during packaging filling, thereby better meeting various chip filling requirements, which can be electronic device potting, board-level CUF, or chip-level CUF, thereby improving the packaging effect.

[0027] In the embodiment of the present application, the visible light transmittance of the slurry is 40%-50%. The epoxy resin used in the epoxy resin system slurry itself does not have high transparency and has a certain haze. The epoxy resin system slurry finally has a high visible light transmittance, indicating that the particle distribution in the system is relatively uniform.

[0028] In the embodiment of the present application, the epoxy resin accounts for 50%-65% by mass in the slurry. Suitable epoxy resin content can enable the slurry to meet the basic physical properties of packaging, achieve filling, and better ensure strong bonding between the chip, solder bumps and substrate.

[0029] In the embodiment of the present application, the mass proportion of the silica modified particles in the slurry is 30%-50%. By controlling the content of the silica modified particles to a higher level, it is beneficial to obtain a lower viscosity of the slurry, obtain better dispersibility and stability, so that the slurry can be used as a bottom filling material, better meet the narrow gap filling requirements, and better improve the problem of particle sedimentation, thereby improving packaging reliability.

[0030] The fifth aspect of the embodiment of the present application provides a slurry, which includes an organic silicon material and the silica-modified particles in the dispersion described in the first aspect of the embodiment of the present application or the silica-modified particles in the dispersion prepared by the preparation method described in the second aspect.

[0031] The slurry provided in the embodiment of the present application is a silicone system slurry, which is obtained by mixing the dispersion of the first aspect of the embodiment of the present application with the silicone material and removing the organic solvent. The residual amount of the organic solvent in the obtained slurry is less than 1%. The obtained slurry has the characteristics of high solid content, high transparency and low viscosity, and can be used for the preparation of optical products, so that the optical products can obtain excellent optical properties while obtaining good processability and mechanical properties.

[0032] In the embodiment of the present application, when the solid content of the slurry is 35%-50%, the visible light transmittance is 80%-97%.

[0033] In the embodiment of the present application, the room temperature viscosity of the slurry is not higher than 5 Pa·s. The slurry has a relatively low viscosity at room temperature, and can obtain good fluidity, which is conducive to molding into optical products of various shapes and sizes, and improving product quality.

[0034] A sixth aspect of the present application provides a method for preparing a slurry, comprising the following steps:

[0035] Alkoxysilane is used as a silicon source and ammonia water is used as a catalyst to obtain a silica particle dispersion by reaction in alcohol and water;

[0036] The silicon dioxide particle dispersion is first subjected to a solvent replacement treatment using an organic solvent, and then the silicon dioxide particles are modified using an alkoxysilane containing an aromatic group to obtain a dispersion; or

[0037] Firstly, the silica particles in the silica particle dispersion are modified by using an alkoxysilane containing an aromatic group, and then a solvent replacement treatment is performed by using an organic solvent to obtain a dispersion; the dispersion comprises silica modified particles and the organic solvent, and the silica modified particles comprise silica particles modified by the alkoxysilane containing an aromatic group;

[0038] The dispersion is mixed with epoxy resin or silicone material to obtain slurry.

[0039] The preparation method of the slurry provided in the embodiment of the present application adopts a liquid phase method and introduces solvent replacement to obtain a dispersion containing modified silica particles, which can significantly reduce the amount of solvent used, and the reaction conditions of the entire preparation process are mild, and a uniform dispersion effect can be achieved without introducing a dispersant or a dispersant. In addition, the preparation process does not introduce metal ions or halogens, and the dispersion has high purity. The dispersion has good dispersibility and high transparency, and can be directly mixed with epoxy resin, silicone material, etc. to obtain a slurry that meets different application requirements.

[0040] The seventh aspect of the embodiment of the present application provides the application of the slurry described in the fourth aspect of the embodiment of the present application in electronic packaging, as well as the application in coating materials, functional film materials, adhesives, and fillers. The epoxy resin system slurry provided in the embodiment of the present application has the characteristics of good dispersibility, good stability, low viscosity, etc., and is applied in the above fields to effectively improve the quality of the obtained products and improve the service reliability of the products.

[0041] In the embodiment of the present application, the application of the slurry in electronic packaging includes the use of the slurry as a bottom filling material for chip packaging. For example, it can be electronic device potting, or it can be board-level CUF (Capillary Underfill), or it can be chip-level CUF. In some embodiments, the slurry is filled between the substrate and the electronic components, and a firm filling layer is formed after heating and curing, which can reduce the stress impact caused by the difference in thermal expansion coefficient between the electronic components and the substrate, improve the strength and connection reliability of the packaging structure, and enhance the overall anti-drop performance of the packaging structure.

[0042] The eighth aspect of the present application provides a packaging device, which includes the cured product of the slurry described in the fourth aspect of the present application. The packaging device of the present application embodiment includes the cured product of the epoxy resin system slurry, which is conducive to improving the reliability of the packaging device.

[0043] In an embodiment of the present application, the packaging device includes a substrate, an electronic component arranged on the substrate, a plurality of solder bumps are arranged on a surface of the electronic component facing the substrate, a bottom filling layer is arranged between the solder bumps, and the bottom filling layer includes the solidified material. In an embodiment of the present application, the packaging device also includes a plastic package covering the surface of the electronic component. In the present application, the electronic component includes but is not limited to a chip. When the electronic component is a chip, the packaging device is a chip packaging structure.

[0044] The present application also provides a terminal device, which includes a circuit board and a packaging device as described in the eighth aspect of the present application, arranged on the circuit board. The terminal device of the present application adopts the packaging device provided by the present application to improve the service reliability of the terminal device.

[0045] The embodiment of the present application further provides a communication device, the communication device comprising the packaging device according to the eighth aspect of the embodiment of the present application. The terminal device of the embodiment of the present application adopts the packaging device provided by the embodiment of the present application to improve the service reliability of the communication device.

[0046] The present application also provides a communication base station, which includes the packaging device described in the eighth aspect of the present application. The communication base station of the present application adopts the packaging device provided by the present application to improve the service reliability of the communication base station.

[0047] The present application also provides the use of the slurry described in the fifth aspect of the present application in optical products, coating materials, medical products, electronic product manufacturing, and building materials. The organic silicon system slurry provided in the present application has the characteristics of good dispersibility, good stability, low viscosity, high transparency, etc., and can be effectively improved in the above fields. BRIEF DESCRIPTION OF THE DRAWINGS

[0048] Figure 1 A schematic diagram of the structure of a packaging device 100 provided in one embodiment of the present application;

[0049] Figure 2 This is a schematic diagram of a packaged device 100 according to an embodiment of the present application being disposed on a circuit board;

[0050] Figure 3 A schematic diagram of the structure of a terminal device 200 provided in an embodiment of the present application;

[0051] Figure 4 This is a SEM (Scanning Electron Microscope) image of modified silica particles in the dispersion prepared in Example 1 of the present application;

[0052] Figure 5 This is a particle size distribution diagram of modified silicon dioxide particles in the dispersion prepared in Example 1 of the present application;

[0053] Figure 6 This is a physical photo of the epoxy resin nano-silica slurry prepared in Example 1 of the present application;

[0054] Figure 7 This is a SEM image of the epoxy resin nano-silica slurry prepared in Example 1 of the present application;

[0055] Figure 8 This is a SEM image of a chip after dispensing with the epoxy resin nano-silicon dioxide slurry prepared in Example 1 of the present application;

[0056] Fig. 9 This is a physical photo of the silicone oil nano-silicon dioxide slurry prepared in Example 3 of the present application;

[0057] Fig.10 This is a physical photo of the DMF nano-silica dispersion prepared in Example 4 of the present application. DETAILED DESCRIPTION

[0058] The embodiments of the present application will be described below in conjunction with the drawings in the embodiments of the present application.

[0059] Filling the packaging material between the substrate and the chip to form a firm bottom filling glue layer after thermal curing can reduce the stress impact caused by the difference in thermal expansion coefficient between the chip and the substrate, protect the chip, substrate and welding bumps, improve the strength and connection reliability of the packaging structure, and enhance the overall anti-drop performance of the packaging structure. In order to increase the number of I / Os and shorten the signal transmission distance in the current advanced packaging structure, the packaging gap is getting smaller and smaller, and the packaging interface is becoming more and more complex. Therefore, the packaging material is required to have good fluidity and low viscosity to better match the increasingly narrow and increasingly complex packaging requirements in the field of electronic packaging. At the same time, it can better avoid the problem of uneven performance of the bottom filling glue layer due to particle sedimentation, which affects the packaging reliability. Based on this, the embodiment of the present application provides a dispersion liquid, and a slurry prepared using the dispersion liquid.

[0060] An embodiment of the present application provides a dispersion, which is a silica dispersion. The dispersion includes modified silica particles and an organic solvent. The modified silica particles include alkoxysilane-modified silica particles containing an aromatic group.

[0061] The dispersion provided in the embodiment of the present application contains silica particles modified by alkoxysilane containing an aromatic group. The present application uses alkoxysilane containing an aromatic group to modify the silica particles, thereby effectively improving the dispersibility of the silica particles in the dispersion, and improving the stability and transparency of the dispersion. The dispersion can then be mixed with an epoxy resin to prepare a slurry with high solid content, high dispersion and low viscosity, which is used as a bottom filling material. While obtaining low viscosity and thixotropy, the problem of particle sedimentation can be effectively improved to improve the packaging effect and the reliability of electronic devices. The dispersion can also be mixed with an organic silicon material to prepare a slurry with high solid content, high transparency and low viscosity, which is used for the preparation of optical products, so that the optical products have good processability and mechanical properties while obtaining excellent optical properties.

[0062] In the embodiment of the present application, the number of carbon atoms of the alkoxysilane containing an aromatic group is less than or equal to 18. In some embodiments, the number of carbon atoms of the alkoxysilane containing an aromatic group may be 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18. A smaller number of carbon atoms can make the structure of the modifying group simpler, the raw material of the modifier is easier to obtain, and it is easier to modify the silica particles.

[0063] In the embodiment of the present application, the molecular weight of the alkoxysilane containing an aromatic group is less than or equal to 600. In some embodiments, the molecular weight of the alkoxysilane containing an aromatic group is 100, 150, 180, 200, 250, 300, 400, 500, 600. Controlling the molecular weight of the alkoxysilane containing an aromatic group to a smaller value can better control the size of the modified group on the surface of the modified silica particles, and is also beneficial to avoid steric hindrance affecting the modification effect.

[0064] In some embodiments of the present application, the alkoxysilane containing aromatic groups can be one or more of methoxysilane containing aromatic groups, ethoxysilane containing aromatic groups, propoxysilane containing aromatic groups, and butoxysilane containing aromatic groups. The aromatic group can be a substituted or unsubstituted phenyl, a substituted or unsubstituted naphthyl, etc. In some embodiments, the alkoxysilane containing aromatic groups is one or more of phenyltrimethoxysilane, phenyltri(dimethylsiloxane)silane, phenyltriethoxysilane, and phenyltri(trimethylsiloxane)silane. The alkoxysilane containing aromatic groups can be chemically bonded to the surface of silica particles to reduce the amount of active hydroxyl groups on the surface of silica particles, and can effectively improve the hydrophobic properties of silica particles, thereby improving the dispersibility and stability of silica dispersion.

[0065] In the embodiment of the present application, in the silica modified particles, the weight proportion of the modified groups derived from the alkoxysilane containing aromatic groups is 20%-45%. In some embodiments, in the silica modified particles, the weight proportion of the modified groups derived from the alkoxysilane containing aromatic groups is 20%, 25%, 30%, 35%, 40%, 45%. Controlling the binding amount of the modified groups on the silica modified particles within a suitable range can better improve the dispersibility of the silica particles in the dispersion, while better avoiding the occurrence of gelation, and improving the stability and transparency of the dispersion.

[0066] In the embodiment of the present application, the organic solvent includes one or more of N,N-dimethylformamide, ketone solvents, ester solvents, and benzene solvents. Among them, the ester solvents can include, for example, methyl formate, ethyl formate, propyl formate, isopropyl formate, butyl formate, isobutyl formate, pentyl formate, isopentyl formate, benzyl formate, hexyl formate, trimethyl orthoformate [trimethoxymethane], methyl acetate, ethyl acetate, vinyl acetate, propyl acetate, isopropyl acetate, allyl acetate [allyl acetate], butyl acetate, isobutyl acetate, sec-butyl acetate, tert-butyl acetate, pentyl acetate, isopentyl acetate, hexyl acetate, etc., and the ketone solvents can include, for example, methyl formate, ethyl formate, propyl formate, isopropyl formate, butyl formate, isobutyl acetate, sec-butyl acetate, tert-butyl acetate, pentyl acetate, isopentyl acetate, hexyl acetate, etc. For example, it can be acetone, methyl acetone, butanone, 2-pentanone, 3-pentanone, acetylacetone [2,4-pentanedione], 3-methyl-2-butanone, 2-hexanone, 3-hexanone, 2-methyl-3-pentanone, 3,3-dimethyl-2-butanone [pinacolone], 4-methyl-2-pentanone, 2-heptanone, 3-heptanone, 4-heptanone, 2,4-dimethyl-3-pentanone, 2-octanone, 5-methyl-3-heptanone, 2,6-dimethyl-4-heptanone, etc., and the benzene solvent can include toluene, for example. The organic solvent can be selected according to the needs of the application and the system requirements. For example, if the dispersion is subsequently mixed with an epoxy resin to prepare a slurry, the organic solvent can be selected as a good solvent for the epoxy resin, such as ethyl acetate.

[0067] In the embodiment of the present application, the dispersion does not contain water. The dispersion of the present application does not contain water, which is beneficial to improving the dispersibility of the modified silica particles and can effectively avoid the introduction of water affecting the reliability verification of subsequent devices.

[0068] In the embodiment of the present application, the dispersion does not contain metal ions. In the embodiment of the present application, the dispersion does not contain halogens. In the bottom filling material, the presence of impure metal ions and halogens will corrode the metal circuits of the chip and have a serious impact on the chip reliability. The silica dispersion of the present application does not contain metal ions and halogens. Using it as a filler for the preparation of the bottom filling material can effectively avoid the impact of metal ion impurities and halogen impurities on the reliability of the package.

[0069] In the embodiment of the present application, the particle size D50 of the silica modified particles is 10nm-100nm. For example, the particle size D50 of the silica modified particles is 10nm, 15nm, 18nm, 20nm, 25nm, 30nm, 35nm, 40nm, 45nm, 50nm, 55nm, 60nm, 65nm, 70nm, 85nm, 90nm, 95nm, 100nm. The particle size of the suitable silica modified particles is conducive to its uniform dispersion in the dispersion liquid, and is also conducive to its use in the bottom filling material, better achieving complete filling, and effectively preventing sedimentation, and improving packaging reliability.

[0070] In some embodiments of the present application, the particle size D10 of the silica modified particles is 16nm-35nm, D50 is 20nm-50nm, and D90 is 35nm-60nm. In some embodiments, the particle size D10 of the silica modified particles is 16nm, 18nm, 20nm, 25nm, 30nm, 35nm. In some embodiments, the particle size D50 of the silica modified particles is 20nm, 25nm, 30nm, 35nm, 40nm, 45nm, 50nm. In some embodiments, the particle size D90 of the silica modified particles is 35nm, 40nm, 45nm, 50nm, 55nm, 60nm. The particle size of silica is relatively uniform and the particle size distribution is narrow, which is conducive to improving the uniformity of the dispersion.

[0071] The particle sizes D10, D50 and D90 of the modified silica particles can be obtained by dynamic light scattering particle size analyzer (DLS).

[0072] In the embodiment of the present application, in the dispersion, the particle size distribution coefficient P of the silica-modified particles is in the range of 0.07-0.17, wherein P = (D90-D10) / D50. In some embodiments, in the dispersion, the particle size distribution coefficient P of the silica-modified particles is 0.07, 0.08, 0.10, 0.12, 0.14, 0.15, 0.16, 0.17. The particle size distribution coefficient of the silica-modified particles is within this range, which can better improve the dispersibility of the dispersion.

[0073] In the embodiment of the present application, the dispersion is a monodisperse system. A monodisperse system refers to a dispersion system with a single dispersed phase and a narrow particle size distribution, and the particle size distribution is normal distribution or approximately normal distribution.

[0074] In the embodiment of the present application, when the solid content of the dispersion is 35%-50%, the visible light transmittance is 80%-99%. Among them, the solid content can be but not limited to 35%, 40%, 45%, 50%, and the visible light transmittance can be but not limited to 80%, 85%, 90%, 95%, 98%, 99%. The solid content is calculated as the proportion of the total mass of the modified silica particles in the dispersion relative to the total mass of the dispersion. The visible light transmittance of the dispersion can be measured by a spectrophotometer. The silica dispersion of the embodiment of the present application, by modifying the silica particles with an alkoxysilane containing an aromatic group, can effectively improve the dispersibility of the silica particles in the dispersion, improve the transparency of the dispersion, and make it conducive to application scenarios with high requirements for transparency.

[0075] In the embodiment of the present application, the dispersion liquid uses alkoxysilane as a silicon source and ammonia water as a catalyst to synthesize silica particles in alcohol and water, and then uses the organic solvent for solvent replacement, and uses the alkoxysilane containing an aromatic group to modify the silica particles. The dispersion liquid of the present application is prepared by the above process, which can reduce the amount of solvent used, and the reaction conditions are mild. A uniform dispersion effect can be achieved without introducing a dispersant or a dispersant; and the process does not introduce metal ions or halogens, and the dispersion liquid has high purity; the dispersion liquid can be applied to a variety of systems.

[0076] An embodiment of the present application provides a method for preparing a dispersion, comprising the following steps:

[0077] Step (1): using alkoxysilane as a silicon source and ammonia water as a catalyst to react in alcohol and water to obtain a silica particle dispersion;

[0078] Wherein, alkoxysilane can be, for example, tetraethoxysilane, i.e., tetraethyl orthosilicate (TEOS), or methyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane, and polysiloxane. Alcohol can be methanol, ethanol, isopropanol, n-butanol, etc. The reaction temperature during the reaction can be controlled within the range of 60°C-70°C, such as 60°C, 65°C, 70°C, and the reaction time can be 4-8 hours, such as 4 hours, 6 hours, 8 hours. Stirring operation can be performed during the reaction, and the stirring speed is controlled within the range of 200rpm-600rpm.

[0079] Wherein, relative to the amount of alcohol, the amount of water can be 1mol / L-6mol / L, the amount of ammonia water can be 0.1mol / L-3mol / L, and the amount of alkoxysilane can be 0.05mol / L-3mol / L. In some embodiments, the amount of water can be 1mol / L, 2mol / L, 3mol / L, 4mol / L, 5mol / L, 6mol / L. In some embodiments, the amount of ammonia water can be 0.1mol / L, 0.3mol / L, 0.5mol / L, 0.7mol / L, 0.9mol / L, 1mol / L, 1.5mol / L, 2mol / L, 2.5mol / L, 3mol / L. In some embodiments, the amount of alkoxysilane used can be 0.05 mol / L, 0.1 mol / L, 0.2 mol / L, 0.3 mol / L, 0.5 mol / L, 0.7 mol / L, 0.9 mol / L, 1 mol / L, 1.5 mol / L, 2 mol / L, 2.5 mol / L, or 3 mol / L.

[0080] Before the solvent replacement treatment in step (2), the method further comprises concentrating the silica particle dispersion obtained in step (1) at a first temperature. The first temperature may be in the range of 40°C to 50°C.

[0081] Step (2): first subjecting a silica particle dispersion to solvent replacement treatment with an organic solvent, and then modifying the silica particles with an alkoxysilane containing an aromatic group to obtain a dispersion; the obtained dispersion includes silica modified particles and an organic solvent, and the silica modified particles include silica particles modified with an alkoxysilane containing an aromatic group.

[0082] The organic solvent can be selected according to actual needs, and can be one or more of N,N-dimethylformamide, ketone solvents, ester solvents, and benzene solvents, as described above. For example, if the dispersion is subsequently mixed with epoxy resin to prepare a slurry, the organic solvent can be a good solvent for epoxy resin, such as ethyl acetate.

[0083] After the solvent replacement treatment is completed, a concentration treatment may be performed first, and then the silica particles may be modified with an alkoxysilane containing an aromatic group. The temperature of the concentration treatment may be in the range of 40° C. to 50° C. When the silica particles are modified with an alkoxysilane containing an aromatic group, the pH of the system after the solvent replacement treatment and the concentration treatment is adjusted to 9-10 with aqueous ammonia.

[0084] Another embodiment of the present application provides a method for preparing a dispersion, comprising the following steps:

[0085] Step (1): using alkoxysilane as a silicon source and ammonia water as a catalyst to react in alcohol and water to obtain a silica particle dispersion;

[0086] Wherein, alkoxysilane can be, for example, tetraethoxysilane, i.e., tetraethyl orthosilicate (TEOS), or methyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane, and polysiloxane. Alcohol can be methanol, ethanol, isopropanol, n-butanol, etc. The reaction temperature during the reaction can be controlled within the range of 60°C-70°C, such as 60°C, 65°C, 70°C, and the reaction time can be 4-8 hours, such as 4 hours, 6 hours, 8 hours. Stirring operation can be performed during the reaction, and the stirring speed is controlled within the range of 200rpm-600rpm.

[0087] Wherein, relative to the amount of alcohol, the amount of water can be 1mol / L-6mol / L, the amount of ammonia water can be 0.1mol / L-3mol / L, and the amount of alkoxysilane can be 0.05mol / L-3mol / L. In some embodiments, the amount of water can be 1mol / L, 2mol / L, 3mol / L, 4mol / L, 5mol / L, 6mol / L. In some embodiments, the amount of ammonia water can be 0.1mol / L, 0.3mol / L, 0.5mol / L, 0.7mol / L, 0.9mol / L, 1mol / L, 1.5mol / L, 2mol / L, 2.5mol / L, 3mol / L. In some embodiments, the amount of alkoxysilane used can be 0.05 mol / L, 0.1 mol / L, 0.2 mol / L, 0.3 mol / L, 0.5 mol / L, 0.7 mol / L, 0.9 mol / L, 1 mol / L, 1.5 mol / L, 2 mol / L, 2.5 mol / L, or 3 mol / L.

[0088] Step (2): first modifying the silica particles in the silica particle dispersion with an aromatic alkoxysilane, and then performing solvent replacement treatment with an organic solvent to obtain a dispersion; the obtained dispersion includes modified silica particles and an organic solvent, and the modified silica particles include silica particles modified with an aromatic alkoxysilane.

[0089] The organic solvent can be selected according to actual needs, and can be one or more of N,N-dimethylformamide, ketone solvents, ester solvents, and benzene solvents, as described above. For example, if the dispersion is subsequently mixed with epoxy resin to prepare a slurry, the organic solvent can be a good solvent for epoxy resin, such as ethyl acetate.

[0090] After the modification is completed, a concentration treatment may be performed first, and then a solvent replacement treatment may be performed. The temperature of the concentration treatment may be in the range of 40° C. to 50° C. The concentration treatment is a reduced pressure concentration treatment performed under vacuum conditions.

[0091] The method for preparing a dispersion provided in an embodiment of the present application adopts a liquid phase method and introduces solvent replacement to obtain a dispersion containing modified silica particles, which can significantly reduce the amount of solvent used, and the reaction conditions of the entire preparation process are mild, and a uniform dispersion effect can be achieved without introducing a dispersant or a dispersant aid; and the preparation process does not introduce metal ions or halogens, and the dispersion has high purity; the dispersion has good dispersibility and high transparency, and can be applied to a variety of systems to meet different application requirements.

[0092] The dispersion provided in the above embodiment of the present application or the dispersion prepared by the above preparation method can be applied to the fields of electronic product manufacturing, optical products, coating materials, functional film materials, adhesives, fillers, medical products, building materials, nanomaterial manufacturing, environmental protection engineering, etc. In the dispersion of the embodiment of the present application, the silicon dioxide particles have good dispersibility, and the dispersion has high stability and transparency. It can be used as a basic raw material and is applicable to a variety of systems to meet different application requirements.

[0093] An embodiment of the present application provides a slurry, which includes epoxy resin and the silicon dioxide modified particles in the dispersion liquid described in the embodiment of the present application.

[0094] The slurry provided in the embodiment of the present application is an epoxy resin system slurry, which is obtained by mixing the dispersion liquid in the embodiment of the present application with epoxy resin and removing the organic solvent, and the residual amount of organic solvent in the obtained slurry is less than 1%. The obtained slurry has the characteristics of high solid content, high dispersion and low viscosity, and is used for bottom filling materials. While obtaining low viscosity and low thixotropy, it can effectively improve the problem of particle sedimentation, improve the packaging effect, and improve the reliability of electronic devices.

[0095] In the embodiment of the present application, the room temperature viscosity of the slurry is lower than 30 Pa·s, and the viscosity at 110°C is lower than 0.075 Pa·s. The slurry has a relatively low viscosity at both room temperature and 110°C, which is conducive to ensuring that the slurry has good fluidity and filling properties during packaging filling, thereby better meeting various chip filling requirements, which can be electronic device potting, board-level CUF, or chip-level CUF, thereby improving the packaging effect.

[0096] The slurry in the embodiment of the present application can be stored at room temperature, which is convenient for storage.

[0097] In the embodiment of the present application, the visible light transmittance of the slurry is 40%-50%. The epoxy resin used in the epoxy resin system slurry itself does not have high transparency and has a certain haze. The high visible light transmittance of the epoxy resin system slurry finally indicates that the particle distribution in the system is relatively uniform.

[0098] In the embodiments of the present application, the epoxy resin may be one or more of a glycidyl ether epoxy resin, a glycidyl ester epoxy resin, a glycidyl amine epoxy resin, an aliphatic epoxy resin, a bisphenol F epoxy resin, a naphthalene epoxy resin, an aminophenol epoxy resin, a binaphthyl epoxy resin, a bisphenol A epoxy resin, and a phenolic epoxy resin. In the resin composition, the epoxy resin may be one or a combination of multiple (two or more). In some embodiments of the present application, the epoxy resin includes one or more of a bisphenol F epoxy resin, an aminophenol epoxy resin, a bisphenol A epoxy resin, a naphthalene epoxy resin, and a binaphthyl epoxy resin.

[0099] In the embodiment of the present application, the mass proportion of epoxy resin in the slurry is 50%-65%. In some embodiments, the mass proportion of epoxy resin is 50%, 52%, 55%, 60%, 62%, 65%. The appropriate epoxy resin content can enable the slurry to meet the basic physical properties of the package, achieve filling, and better ensure the strong bonding between the chip, the solder bump and the substrate.

[0100] In the embodiment of the present application, the mass proportion of silica modified particles in the slurry is 30%-50%. In some embodiments, the mass proportion of silica modified particles in the slurry is 30%, 35%, 40%, 45%, 50%. By controlling the content of silica modified particles to a higher level, it is beneficial to make the slurry have a lower viscosity, better dispersibility and stability, so that the slurry can be used as a bottom filling material, better meet the needs of narrow gap filling, and better improve the problem of particle sedimentation and improve packaging reliability.

[0101] In some embodiments of the present application, other resin materials other than epoxy resin may be added to the slurry as needed, and other inorganic fillers other than silica may be added as needed.

[0102] In the embodiment of the present application, an epoxy resin system slurry prepared by using silica modified with alkoxysilane containing an aromatic group is used in bottom filling, and the thermal expansion coefficient, glass transition temperature, and mechanical properties such as TMA (thermomechanical analysis) and DMA (dynamic thermomechanical analysis) of the entire system can meet the physical property requirements.

[0103] In the embodiment of the present application, when used for the bottom filling material, the slurry is added to the bottom filling glue system, and the bottom filling glue system may include a curing agent. The curing agent may include an amine curing agent and / or an anhydride curing agent. In the embodiment of the present application, the anhydride curing agent may be one or more of hexahydrophthalic anhydride, tetrahydrophthalic anhydride, methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, hexahydrophthalic anhydride, alkylhexahydrophthalic anhydride, tetrahydrophthalic anhydride, succinic anhydride, methylnadic anhydride, hydrogenated methylnadic anhydride, 5-norbornene-2,3-dianhydride, trialkyltetrahydrophthalic anhydride, etc. In the embodiment of the present application, the amine curing agent may be an aromatic amine curing agent or an aliphatic amine curing agent, wherein the amine curing agent may be, for example, diethyltoluenediamine, polyetheramine, isophoronediamine, 3,3'-dimethyl-4,4'-diamino-dicyclohexylmethane, etc. The bottom filling glue system may also include additives, including one or more of a coupling agent, a stress modifier, a curing accelerator, a colorant, a dispersant, an ion trap, a leveling agent, a flame retardant, a release agent, and a flow improver. It is understandable that the additives may be added according to specific needs.

[0104] The present application also provides the application of the above slurry in electronic packaging, as well as the application in coating materials, functional film materials, adhesives, and fillers. The slurry in this embodiment has the characteristics of good dispersibility, good stability, and low viscosity. When applied to the above fields, it can effectively improve the quality of the obtained products and improve the service reliability of the products.

[0105] In the embodiments of the present application, the application of the slurry in electronic packaging includes the use of the slurry as a bottom filling material for chip packaging. For example, it can be electronic device potting, board-level CUF, or chip-level CUF. In some embodiments, the slurry is filled between the substrate and the electronic components, and a firm filling layer is formed after heating and curing, which can reduce the stress impact caused by the difference in thermal expansion coefficient between the electronic components and the substrate, improve the strength and connection reliability of the packaging structure, and enhance the overall anti-drop performance of the packaging structure.

[0106] In the embodiment of the present application, the electronic components can be chips, transistors (such as diodes, triodes), LEDs, RC-sensing elements (such as resistors, capacitors, inductors), etc. The structural form of the package can be advanced packaging structures such as flip chip, fan-in wafer-level package FOWLP, fan-out wafer-level package FOWLP, through silicon via technology TSV, 2.5D packaging, 3D packaging, embedded wafer-level ball grid array package eWLB, etc., and can also be packaging structures such as large-area molding, thin-type packaging without grinding, passive device packaging, and POP (package-on-package, package stacking technology) packaging. The epoxy resin system slurry provided in the embodiment of the present application is a liquid packaging material, which has good packaging filling ability and can better meet the packaging requirements of advanced packaging structures.

[0107] See also Figure 1 The present application also provides a packaging device 100. Figure 1 1 is a schematic diagram of the structure of a packaged device 100 in one embodiment of the present application. The packaged device 100 may be an electronic device package, and the packaged device 100 includes the cured product of the epoxy resin system slurry described above in the embodiment of the present application. The packaged device 100 in the embodiment of the present application includes the cured product of the epoxy resin system slurry described above, which is beneficial to improving the reliability of the packaged device.

[0108] In some embodiments of the present application, the packaging device 100 includes a substrate 10, an electronic component 20 disposed on the substrate 10, a plurality of solder bumps 30 are disposed on the surface of the electronic component 20 facing the substrate 10, and a bottom filling glue layer 40 is disposed between the soldering bumps 30, that is, between the substrate 10, the electronic component 20, and the soldering bumps 30, and the bottom filling glue layer 40 includes the cured product of the epoxy resin system slurry described in the embodiment of the present application. In the embodiment of the present application, the packaging device 100 also includes a plastic package 60 covering the surface of the electronic component 20. In the embodiment of the present application, the soldering bump 30 is electrically connected to the electronic component 20 through the conductive structure 50 in the substrate 10. Among them, the electronic component 20 can be various components that need to be packaged, including but not limited to one or more of chips, transistors (such as diodes, triodes), LEDs, resistors, capacitors, and inductors (such as resistors, capacitors, inductors), etc. When the electronic component 20 is a chip, the packaging device 100 is a chip packaging structure. The electronic component 20 may be attached to the surface of the substrate 10 by soldering, and the substrate 10 may be a redistribution layer (RDL). Figure 2The packaged device 100 can be soldered to the circuit board 101, and a plurality of metal balls 70 can be arranged on the side of the substrate 10 away from the electronic components 20. The electronic components 20 in the packaged device 100 can be electrically connected to the circuit board 101 through the conductive structure 50 and the metal balls 70. A filling adhesive layer 80 is provided between the substrate 10, the circuit board 101 and the metal balls 70. The filling adhesive layer 80 can also be a cured product including the epoxy resin system slurry described above in the embodiment of the present application.

[0109] The packaged device 100 of the embodiment of the present application uses the epoxy resin system slurry provided in the embodiment of the present application to package electronic components, and has good filling properties, high process operability, and high packaging reliability.

[0110] See also Figure 3 The embodiment of the present application further provides a terminal device 200, the terminal device 200 includes a housing 201 and a circuit board and a packaging device 100 disposed in the housing 201. Inside the terminal device 200, the packaging device 100 may be as follows Figure 2 As shown, it is arranged on the circuit board 101 and is electrically connected to the circuit board 101. The terminal device 200 can be a mobile phone, a tablet computer, a laptop computer, a portable machine, a smart wearable product, a television, a video recorder, a camcorder, a radio, a radio recorder, a vehicle terminal, a mouse, a keyboard, a microphone, a scanner, etc. The terminal device of the embodiment of the present application adopts the packaging device provided by the embodiment of the present application to improve the service reliability of the terminal device.

[0111] The embodiment of the present application also provides a communication device, which includes the packaged device 100 described above in the embodiment of the present application. The packaged device 100 can be electrically connected and fixed on a circuit board. The communication device can be various types of wired communication devices or wireless communication devices, including but not limited to communication conversion devices, lightning arresters, antennas, gateways, remote controls, radars, intercoms, switches, routers, etc. The terminal device of the embodiment of the present application adopts the packaged device provided in the embodiment of the present application to improve the service reliability of the communication equipment.

[0112] The present application also provides a communication base station, which includes the packaging device 100 described above in the present application. The packaging device 100 can be electrically connected and fixed on a circuit board. The communication base station of the present application adopts the packaging device provided in the present application to improve the service reliability of the communication base station.

[0113] Another embodiment of the present application provides a slurry, which includes an organosilicon material and the silicon dioxide modified particles in the dispersion liquid described in the embodiment of the present application, and is an organosilicon system slurry.

[0114] The silicon bonds in the organosilicon system are very weak, which leads to its generally poor mechanical properties. In order to enhance the mechanical strength and rigidity of the organosilicon system so that it can meet the application requirements of high-performance coatings, adhesives and composite materials, it is usually necessary to add some inorganic fillers such as silica for reinforcement. However, in certain application scenarios, such as automotive glass, optical materials and other optical products, it is hoped that the transparency of the system will not be affected while reinforcement is performed. The slurry provided in the embodiment of the present application is an organosilicon system slurry, which is prepared by mixing the above-mentioned dispersion of the embodiment of the present application with an organosilicon material and removing the organic solvent. The residual amount of organic solvent in the obtained slurry is less than 1%. The obtained slurry has the characteristics of high solid content, high transparency and low viscosity, and can be used for the preparation of optical products, so that the optical products can obtain excellent optical properties while obtaining good processability and mechanical properties.

[0115] In the embodiment of the present application, the organosilicon material is a liquid organosilicon material, and the organosilicon material can be a silicone oil type organosilicon material. The silicone oil type organosilicon material can be ordinary silicone oil, i.e. methyl silicone oil, or it can be a modified silicone oil. In some embodiments, the modified silicone oil can be one or more of epoxy-modified silicone oil, polyether-modified silicone oil, and amino-modified silicone oil. Epoxy-modified silicone oil is a type of silicone oil containing epoxy groups in the side chains or end groups of polydimethylsiloxane. Polyether-modified silicone oil is a polydimethylsiloxane containing a polyether group in the side chain or end group, and the polyether group is, for example, polyoxyethylene, polyoxypropylene, and fatty alcohol polyoxyethylene polyoxypropylene ether. Amino-modified silicone oil is a polydimethylsiloxane containing an amino group in the side chain or end group.

[0116] In the embodiment of the present application, when the solid content of the slurry is 35%-50%, the visible light transmittance is 80%-97%. Among them, the solid content can be but not limited to 35%, 40%, 45%, 50%, and the visible light transmittance can be but not limited to 80%, 85%, 90%, 95%, 97%. The solid content is calculated as the proportion of the total mass of the modified silica particles in the slurry relative to the total mass of the slurry. The visible light transmittance of the slurry can be measured by a spectrophotometer. The organosilicon system slurry of the embodiment of the present application has excellent transparency due to the use of a dispersion of silica particles modified by alkoxysilane containing aromatic groups mixed with an organosilicon material, which is beneficial to the application of the slurry in application scenarios with high requirements for transparency.

[0117] In the embodiment of the present application, the room temperature viscosity of the slurry is not higher than 5Pa·s, that is, less than or equal to 5Pa·s. The slurry has a low viscosity at room temperature and can obtain good fluidity, which is conducive to molding into optical products of various shapes and sizes and improving product quality.

[0118] The present application also provides the use of the above-mentioned organosilicon system slurry in optical products, coating materials, medical products, electronic product manufacturing, and building materials. The organosilicon system slurry provided in the present application has the characteristics of good dispersibility, good stability, low viscosity, high transparency, etc., and can be effectively improved in the above-mentioned fields. The performance of the obtained product.

[0119] The present invention also provides a method for preparing a slurry, comprising the following steps:

[0120] Step (1): using alkoxysilane as a silicon source and ammonia water as a catalyst to react in alcohol and water to obtain a silica particle dispersion;

[0121] Step (2): first subjecting the silica particle dispersion to solvent replacement treatment with an organic solvent, and then modifying the silica particles with an alkoxysilane containing an aromatic group to obtain a dispersion; or

[0122] Firstly, the silica particles in the silica particle dispersion are modified by using an alkoxysilane containing an aromatic group, and then a solvent replacement treatment is performed by using an organic solvent to obtain a dispersion; the obtained dispersion comprises silica modified particles and the organic solvent, and the silica modified particles comprise silica particles modified by the alkoxysilane containing an aromatic group;

[0123] Step (3): Mix the dispersion with epoxy resin or silicone material to obtain a slurry.

[0124] Among them, step (1) and step (2) are methods for preparing a dispersion, which are consistent with the above and will not be repeated here. It can be understood that considering that step (3) mixes the dispersion with an epoxy resin or an organosilicon material, the organic solvent used in step (2) for solvent replacement is a good solvent for the epoxy resin or the organosilicon material. A good solvent refers to a solvent with high solubility that can dissolve epoxy resin or organosilicon material well. In some embodiments, the boiling point of the organic solvent is lower than 120°C. The organic solvent has a lower boiling point, which is beneficial to temperature control of the preparation process.

[0125] In step (3), after the dispersion is mixed with the epoxy resin or the organosilicon material, a concentration process is further included, and the temperature of the concentration process is greater than 55° C., for example, 60° C. The concentration process is a reduced pressure concentration process performed under vacuum conditions. The organic solvent can be removed during the concentration process.

[0126] The preparation method of the slurry provided in the embodiment of the present application adopts a liquid phase method and introduces solvent replacement to obtain a dispersion containing modified silica particles, which can significantly reduce the amount of solvent used, and the reaction conditions of the entire preparation process are mild, and a uniform dispersion effect can be achieved without introducing a dispersant or a dispersant aid; and the preparation process does not introduce metal ions or halogens, and the dispersion has high purity; and the dispersion has good dispersibility and high transparency, and can be directly mixed with epoxy resin to obtain a high-solid content, high-dispersion, low-viscosity slurry for bottom filling materials, which can effectively improve the problem of particle sedimentation while obtaining low viscosity and thixotropy, so as to improve the packaging effect and the reliability of electronic devices; it can also be directly mixed with silicone materials to obtain a slurry with high solid content, high transparency, and low viscosity, which is used for the preparation of optical products, so that the optical products have good processability and mechanical properties while obtaining excellent optical properties.

[0127] The embodiments of the present application are further described below with reference to a plurality of embodiments.

[0128] The ionic solid content of the slurry was measured by TGA (Thermo Gravimetric Analyzer), and the test conditions of TGA were 20°C / min from 0°C to 800°C.

[0129] The viscosity of the slurry was measured by rheometer at room temperature and 110°C with a shear rate range of 0-100 1 / s, and the corresponding viscosity value was taken at 501 / s.

[0130] The visible light transmittance of the slurry or dispersion is measured by a UV-visible spectrophotometer at room temperature in the visible light range of 300-800 nm.

[0131] Example 1

[0132] The preparation method of epoxy resin system slurry comprises the following steps:

[0133] (1) Particle formation and solvent replacement:

[0134] Add appropriate amount of deionized water and ammonia water to 1.2L ethanol, mix and stir at 65°C; after the temperature stabilizes, add TEOS, control the stirring speed to 400rpm, react for 6h, and generate silica particles with a D50 particle size of 30±5nm; after the reaction, place the silica reaction liquid at 40°C and concentrate it to 400mL, then add 400mL of ethyl acetate and stir evenly, and then concentrate it to 300mL at 40°C to obtain a silica concentrated liquid.

[0135] (2) Modification:

[0136] Ammonia water was added to the silica concentrate to adjust the pH of the system to 9, 0.5 mL of deionized water was added and stirred evenly, and then 4.8 g of phenyltrimethoxysilane was added and reacted for 6 h to obtain a modified silica sol; then coarse particles were removed by centrifugation, the centrifugal force was controlled to 424Xg, centrifuged for 2 min, and the upper liquid was retained to obtain a dispersion.

[0137] (3) Add epoxy resin:

[0138] Add 24g of epoxy resin dissolved in ethyl acetate to the dispersion, stir for 20min, concentrate and spin out the ethyl acetate at 60°C to obtain a translucent epoxy resin nano-silica slurry with a particle solid content of 36.45%. The room temperature viscosity of the obtained epoxy resin nano-silica slurry is less than 30Pa·s, the high temperature viscosity at 110°C is less than 0.075Pa·s, and the measurement gap is 0.2mm. The fluidity test results of the obtained epoxy resin nano-silica slurry are:

[0139] Figure 4 This is a SEM image of modified silica particles in the dispersion prepared in Example 1 of the present application. Figure 4 It can be seen that in the dispersion prepared in the embodiment of the present application, the particle size of the modified silicon dioxide particles is uniform and small, at the nanometer level. Figure 5 This is a particle size distribution diagram of modified silicon dioxide particles in the dispersion prepared in Example 1 of the present application. Figure 5 It can be seen that in the dispersion prepared in the example of the present application, the particle size of the modified silicon dioxide particles is uniform and narrowly distributed. The figure shows a curve obtained by three parallel measurements, and the peak of the curve is about 30 nm.

[0140] Figure 6 This is a photo of the epoxy resin nano-silicon dioxide slurry prepared in Example 1 of the present application. Figure 6 It can be seen that the epoxy resin nano-silica slurry prepared in the embodiment of the present application is a translucent liquid phase system with good fluidity. Figure 7 This is a SEM image of the epoxy resin nano-silicon dioxide slurry prepared in Example 1 of the present application. Figure 7 It can be seen that in the epoxy resin nano-silica slurry, the modified silica particles are well dispersed without agglomeration.

[0141] The epoxy resin nano-silicon dioxide slurry prepared in Example 1 was prepared into bottom filling glue, and a chip dispensing test was performed. Figure 8 This is a SEM image of a chip slice after glue dispensing using Example 1 of the present application. Figure 8 The results show that the encapsulation using the epoxy resin nano-silica slurry of the present application has no filler phase separation and has a good anti-settling effect.

[0142] Example 2

[0143] The preparation method of epoxy resin system slurry comprises the following steps:

[0144] (1) Particle generation and modification:

[0145] Add appropriate amount of deionized water and ammonia water to 1.2L of ethanol, mix and stir at 65°C; after the temperature stabilizes, add TEOS, control the stirring speed to 400rpm, react for 6h, and generate silica particles with a D50 particle size of 30±5nm; add 5.8g of phenyltrimethoxysilane to the silica reaction solution, react for 6h to obtain modified silica sol.

[0146] (2) Solvent replacement:

[0147] The modified silica sol was concentrated to 400 mL at 40°C, and then 400 mL of ethyl acetate was added and stirred evenly for solvent replacement at 40°C. After the temperature stabilized, it was concentrated to about 300 mL, and then the centrifugal force was controlled at 424Xg and centrifuged for 2 minutes to retain the upper dispersion.

[0148] (3) Add epoxy resin:

[0149] 24g of epoxy resin dissolved in ethyl acetate was added to the dispersion, stirred for 20 minutes, concentrated at 60°C, and ethyl acetate was spun out to obtain a translucent epoxy resin nano-silica slurry with a particle solid content of 38.56%. The room temperature viscosity of the obtained epoxy resin nano-silica slurry was less than 30Pa·s, and the high temperature viscosity at 110°C was less than 0.075Pa·s.

[0150] Example 3

[0151] The method for preparing the organosilicon system slurry comprises the following steps:

[0152] (1) and (2) are the same as in Example 1 or Example 2;

[0153] (3) Add silicone oil:

[0154] Add 20g of organic silicone oil dissolved in ethyl acetate to the dispersion, stir for 20min, concentrate at 60°C and spin out the ethyl acetate to obtain a highly transparent silicone oil nano-silicon dioxide slurry. The solid content of the obtained silicone oil nano-silicon dioxide slurry was measured to be 44.58% under oxygen TGA (Thermo Gravimetric Analyzer, thermal gravimetric analysis). The viscosity of the obtained silicone oil nano-silicon dioxide slurry at room temperature is less than 5Pa·s, and the measurement gap is 0.05mm.

[0155] Table 1 shows the transmittance data of pure silicone oil and silicone oil nano-silica slurry in the visible light wavelength range of 300nm-800nm. All measurements were made three times and the average value was taken. Fig. 9 This is a physical photo of the silicone oil nano-silica slurry prepared in Example 3 of the present application.

[0156] Table 1 Transmission results of pure silicone oil and silicone oil nano-silica slurry

[0157]

[0158] From the results in Table 1, it can be seen that the transmittance of the silicone oil nano-silica slurry in the embodiment of the present application is 94.6% of the transmittance of pure silicone oil, that is, after the modified silica dispersion in the embodiment of the present application is mixed with silicone oil, even at a high solid content, the visible light transmittance of the system will not be significantly reduced, and the silicone oil nano-silica slurry can maintain a high transparency.

[0159] Depend on Fig. 9 It can be seen that the silicone oil nano-silica slurry is a highly transparent liquid phase system with good transparency.

[0160] Example 4

[0161] The preparation method of DMF nano-silicon dioxide dispersion comprises the following steps:

[0162] (1) Particle generation and modification:

[0163] Add 2.8 mol / L (relative to ethanol) of deionized water and 0.6 mol / L (relative to ethanol) of ammonia water to 1.2 L of ethanol, and stir at 65°C; after the temperature stabilizes, add 0.224 mol / L (relative to ethanol) of TEOS, control the stirring speed to 400 rpm, react for 6 hours, and generate silica particles with a D50 particle size of 30±5 nm; add 5.8 g of phenyltrimethoxysilane to the silica reaction solution, and react for 6 hours to obtain a modified silica sol.

[0164] (2) Solvent replacement:

[0165] The modified silica sol was concentrated to 400 mL at 40°C, and then 400 mL of DMF was added and stirred evenly. The solution was concentrated and replaced at 80°C. After the temperature stabilized, the solvent was concentrated to a solution volume of about 300 mL. The solution was then centrifuged at 424Xg for 2 minutes to remove coarse particles and obtain a uniform and transparent DMF silica dispersion.

[0166] Table 2 shows the transmittance data of pure DMF solvent and DMF nano-silica dispersion in the visible light wavelength range of 300nm-800nm. All measurements were made three times and the average value was taken. Fig.10 This is a physical photo of the DMF nano-silica dispersion prepared in Example 4 of the present application.

[0167] Table 2 Transmission results of pure DMF solvent and DMF nano-silica dispersion

[0168]

[0169]

[0170] From the results in Table 2, it can be seen that the transmittance of the DMF nano-silica dispersion in the embodiment of the present application is 99.2% of the transmittance of pure DMF, that is, the modified silica dispersion in the embodiment of the present application does not significantly reduce the visible light transmittance of the system compared to a simple organic solvent.

[0171] Depend on Fig.10 It can be seen that the DMF nano-silica dispersion of the present embodiment has good transparency.

[0172] It should be understood that the first, second and various numerical numbers involved in this document are only distinguished for the convenience of description and are not used to limit the scope of the present application.

[0173] In this application, "and / or" describes the association relationship of associated objects, indicating that there can be three relationships. For example, A and / or B can mean: A exists alone, A and B exist at the same time, and B exists alone, where A and B can be singular or plural. The character " / " generally indicates that the associated objects are in an "or" relationship.

[0174] In this application, "at least one" means one or more, and "plurality" means two or more. "At least one of the following" or similar expressions refers to any combination of these items, including any combination of single items or plural items. For example, "at least one of a, b, or c", or "at least one of a, b, and c" can all mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, c can be single or multiple, respectively.

[0175] In this application, “-” represents a range value, including the endpoint values ​​at both ends. For example, the value of a can be 0.5-15, which means that the value of a can be between 0.5 and 15, and includes the endpoint values ​​0.5 and 15.

[0176] It should be understood that in the various embodiments of the present application, the size of the serial numbers of the above-mentioned processes does not mean the order of execution, some or all of the steps can be executed in parallel or sequentially, and the execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.

Claims

1. A dispersion, characterized in that: The dispersion includes silica-modified particles and an organic solvent, and the silica-modified particles include silica particles modified with alkoxysilane containing an aromatic group.

2. The dispersion according to claim 1, characterized in that The aromatic group-containing alkoxysilane has 18 or less carbon atoms.

3. The dispersion according to claim 1 or 2, characterized in that The molecular weight of the aromatic group-containing alkoxysilane is less than or equal to 600.

4. The dispersion according to any one of claims 1 to 3, characterized in that In the modified silica particles, the weight proportion of the modified groups derived from the aromatic group-containing alkoxysilane is 20%-45%.

5. The dispersion according to any one of claims 1 to 4, characterized in that The organic solvent includes one or more of N,N-dimethylformamide, ketone solvents, ester solvents, and benzene solvents.

6. The dispersion according to any one of claims 1 to 5, characterized in that The dispersion does not contain water.

7. The dispersion according to any one of claims 1 to 6, characterized in that The dispersion does not contain metal ions; or the dispersion does not contain halogens.

8. The dispersion according to any one of claims 1 to 7, characterized in that The particle size D50 of the modified silica particles is 10nm-100nm.

9. The dispersion according to claim 8, characterized in that The particle size D10 of the modified silicon dioxide particles is 16nm-35nm, D50 is 20nm-50nm, and D90 is 35nm-60nm.

10. The dispersion according to claim 9, characterized in that In the dispersion, the particle size distribution coefficient P of the modified silica particles is in the range of 0.07-0.17, wherein P=(D90-D10) / D50.

11. The dispersion according to any one of claims 1 to 10, characterized in that When the solid content of the dispersion is 35%-50%, the visible light transmittance is 80%-99%.

12. The dispersion according to any one of claims 1 to 11, characterized in that The dispersion liquid is obtained by synthesizing silicon dioxide particles in alcohol and water using alkoxysilane as a silicon source and ammonia water as a catalyst, then using the organic solvent for solvent replacement, and using alkoxysilane containing an aromatic group to modify the silicon dioxide particles.

13. A method for preparing a dispersion, comprising the following steps: Alkoxysilane is used as a silicon source and ammonia water is used as a catalyst to obtain a silica particle dispersion by reaction in alcohol and water; The silica particle dispersion is first subjected to solvent replacement treatment with an organic solvent, and then the silica particles are modified with an alkoxysilane containing an aromatic group to obtain a dispersion; or the silica particles in the silica particle dispersion are first modified with an alkoxysilane containing an aromatic group, and then solvent replacement treatment is performed with an organic solvent to obtain a dispersion; the dispersion includes modified silica particles and the organic solvent, and the modified silica particles include silica particles modified with an alkoxysilane containing an aromatic group.

14. Use of the dispersion according to any one of claims 1 to 12 or the dispersion prepared by the preparation method according to claim 13 in the manufacture of electronic products, optical products, coating materials, functional film materials, adhesives, fillers, medical products, building materials, nanomaterials, and environmental protection projects.

15. A slurry, characterized in that: The slurry comprises epoxy resin, and the silicon dioxide modified particles in the dispersion according to any one of claims 1 to 12 or the silicon dioxide modified particles in the dispersion obtained by the preparation method according to claim 13.

16. The slurry according to claim 15, characterized in that The room temperature viscosity of the slurry is lower than 30 Pa·s, and the viscosity at 110° C. is lower than 0.075 Pa·s.

17. The slurry according to claim 15 or 16, characterized in that The visible light transmittance of the slurry is 40%-50%.

18. The slurry according to any one of claims 15 to 17, characterized in that In the slurry, the epoxy resin accounts for 50%-65% by mass; the silicon dioxide modified particles account for 30%-50% by mass.

19. A slurry, characterized in that: The slurry comprises an organic silicon material and the silicon dioxide modified particles in the dispersion according to any one of claims 1 to 12 or the silicon dioxide modified particles in the dispersion obtained by the preparation method according to claim 13.

20. The slurry according to claim 19, characterized in that When the solid content of the slurry is 35%-50%, the visible light transmittance is 80%-97%.

21. The slurry according to claim 19 or 20, characterized in that The room temperature viscosity of the slurry is not higher than 5 Pa·s.

22. A method for preparing a slurry, comprising the following steps: Alkoxysilane is used as a silicon source and ammonia water is used as a catalyst to obtain a silica particle dispersion by reaction in alcohol and water; The silica particle dispersion is first subjected to solvent replacement treatment with an organic solvent, and then the silica particles are modified with an alkoxysilane containing an aromatic group to obtain a dispersion; or the silica particles in the silica particle dispersion are first modified with an alkoxysilane containing an aromatic group, and then the dispersion is subjected to solvent replacement treatment with an organic solvent to obtain a dispersion; the dispersion comprises modified silica particles and the organic solvent, and the modified silica particles comprise silica particles modified with an alkoxysilane containing an aromatic group; The dispersion is mixed with epoxy resin or silicone material to obtain slurry.

23. Use of the slurry according to any one of claims 15 to 18 in electronic packaging, and in coating materials, functional film materials, adhesives and fillers.

24. The use according to claim 23, characterized in that The application of the slurry in electronic packaging includes using the slurry as a bottom filling material for chip packaging.

25. A packaged device, characterized in that: The packaging device comprises a cured product of the slurry according to any one of claims 15 to 18.

26. The packaged device according to claim 25, characterized in that The packaging device comprises a substrate and electronic components arranged on the substrate. A surface of the electronic components facing the substrate is provided with a plurality of solder bumps. A bottom filling adhesive layer is provided between the solder bumps. The bottom filling adhesive layer comprises the solidified material.

27. A terminal device, characterized in that: The terminal device includes a circuit board and a packaging device as claimed in claim 25 or 26 arranged on the circuit board.

28. A communication device, characterized in that: The communication device comprises the packaged device according to claim 25 or 26.

29. A communication base station, characterized in that: The communication base station comprises the packaged device as claimed in claim 25 or 26.

30. Use of the slurry according to any one of claims 19 to 21 in optical products, coating materials, medical products, electronic product manufacturing, and building materials.

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